Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate
Nisoldipine
CAS: 63675-72-9
Molecular Formula: C20H24N2O6
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Names and Identifiers
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Physico-chemical Properties
| Molecular Formula | C20H24N2O6 |
| Molar Mass | 388.41 |
| Density | 1.205±0.06 g/cm3(Predicted) |
| Melting Point | 147-148°C |
| Boling Point | 503.3±50.0 °C(Predicted) |
| Flash Point | 258.2°C |
| Solubility | Soluble in DMSO, insoluble in water |
| Vapor Presure | 2.95E-10mmHg at 25°C |
| Appearance | Yellow to light yellow powder |
| Color | yellow |
| Merck | 14,6565 |
| pKa | 2.67±0.70(Predicted) |
| Storage Condition | room temp |
| Refractive Index | 1.544 |
| MDL | MFCD00478055 |
| Physical and Chemical Properties | Yellow to light yellow powder, odorless and tasteless. Melting Point 151~152 °c (ethanol). |
| Use | Strong calcium antagonists for the treatment of hypertension with coronary heart disease, hypertension and mild heart failure |
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Risk and Safety
| Hazard Symbols | Xn - Harmful |
| Risk Codes | 20/21/22 - Harmful by inhalation, in contact with skin and if swallowed. |
| Safety Description | 36 - Wear suitable protective clothing. |
| WGK Germany | 3 |
| RTECS | US7975600 |
| HS Code | 2933399090 |
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Nature
Open Data Verified Data
yellow to light yellow powder, odorless and tasteless. Crystallization in ethanol, melting point 151~152.
Last Update：2024-01-02 23:10:35
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Preparation Method
Open Data Verified Data
O-nitrobenzaldehyde is reacted with isobutyl acetoacetate to give isobutyl 2-(2-nitrobenzylidene) acetoacetate. The compound and 3 a amino acid methyl benzene in ethanol, heating Reflux reaction. After cooling, the solvent was distilled off under reduced pressure. The obtained oily substance was mixed with a small amount of ethanol, and the crystals were completely precipitated by leaving a small amount. Filtration and recrystallization with ethanol were performed to obtain Nisoldipine.
Last Update：2022-01-01 09:10:22
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Standard
Authoritative Data Verified Data
This product is (±)-2, 6-dimethyl-4-(2-nitrophenyl) -1, 4-dihydro-3, 5-pyridinedicarboxylic acid methyl ester isobutyl ester. Calculated as dried product, the content of C20H24N206 shall not be less than 98.5%.
Last Update：2024-01-02 23:10:35
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Trait
Authoritative Data Verified Data
- This product is yellow crystalline powder; Odorless; Unstable in light.
- This product is soluble in acetone or chloroform, slightly soluble in ethanol, almost insoluble in water.
melting point
The melting point of this product (General 0612) is 148~152°C.
Last Update：2022-01-01 11:42:39
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Use
Open Data Verified Data
developed by Bayer, Germany, launched in January 1989. Dihydropyridine calcium ion antagonists. With selective expansion of coronary artery effect, stronger than nifedipine 4~10 times. Can reduce myocardial oxygen consumption and total peripheral resistance, can also increase coronary collateral circulation, coronary flow increased. Enhance the tolerance of myocardium to hypoxia and reduce blood pressure in hypertensive patients. While causing a drop in blood pressure, there was no significant effect on the respiratory and central nervous system. For hypertension, heart failure, ischemic heart disease, angina pectoris, angina, especially suitable for coronary heart disease with hypertension.
Last Update：2022-01-01 09:10:23
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Differential diagnosis
Authoritative Data Verified Data
- take about 30mg of this product, add 2ml of acetone to dissolve, add 3~5 drops of 20% sodium hydroxide solution, shake, the solution shows orange red.
- light-shielding operation. Take this product, add anhydrous ethanol dissolved and diluted into a solution containing about 10ug per lml, according to ultraviolet-visible spectrophotometry (General 0401) determination, there is maximum absorption at the wavelength of 237mn.
- The infrared absorption spectrum of this product should be consistent with that of the control (Spectrum set 1127).
Last Update：2022-01-01 11:42:40
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Exam
Authoritative Data Verified Data
Related substances
operation in the dark. Take this product, precision weighing, add mobile phase dissolution and quantitative dilution to make a solution containing about 0.4mg per lml, as a test solution; Another 2, 6-dimethyl-4-(2-nitrophenyl)-3, 5-pyridinedicarboxylic acid methyl ester isobutyl ester (impurity I) control and 2, 6-dimethyl-4-(2-nitrosophenyl)-3, 5-pyridinedicarboxylic acid methyl ester isobutyl ester (impurity II) reference, precision weighing, add the mobile phase to dissolve and quantitatively dilute to make a mixed solution containing about 40ug in each lml, take 2ml with precision, put it in a 100ml measuring flask, and add 1ml of human test solution with precision, dilute to the scale with the mobile phase, shake, and serve as a control solution. Test according to high performance liquid chromatography (General 0512). With eighteen alkyl silane bonded silica as filler; Methanol-acetonitrile-water (50:15:35) as mobile phase; The detection wavelength was 237mm, the impurity I reference substance and the impurity n reference substance are dissolved and diluted by adding mobile phase to make a mixed solution containing about 400ug, 1.2ug and 1.2ug in each lml, and then the mixed solution is taken out of LOL and injected into human liquid chromatograph, the degree of separation between the impurity I peak, the impurity II peak and the nisoldine peak shall meet the requirements. The test solution and the control solution were respectively injected into the human liquid chromatograph, and the chromatogram was recorded to 4 times of the retention time of the main component peak. If there are chromatographic peaks in the chromatogram of the test solution that are consistent with the retention time of impurity I peak and impurity II peak, the peak area shall be calculated according to the external standard method, and shall not exceed 0.2%; the Peak area of other individual impurities shall not be greater than 0.5 times (0.5%) The Peak area of Nisoldipine in the control solution; The total amount of impurities shall not exceed 1.5%.
loss on drying
take this product, dry to constant weight at 105°C, weight loss shall not exceed 0.5% (General rule 0831).
ignition residue
take l.Og of this product and check it according to law (General rule 0841). The residue left shall not exceed 0.1%.
Heavy metals
The residue left under the item of taking the ignition residue shall not contain more than 10 parts per million of heavy metal when examined by law (General Principles 0821, Law II).
Last Update：2022-01-01 11:42:41
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Content determination
Authoritative Data Verified Data
take about 0.25g of this product, precision weighing, add glacial acetic acid 20ml and dilute sulfuric acid 10ml, dissolve at a slight temperature, let cool, add 2 drops of adjacent phenanthroline indicator solution, and use cerium sulfate titration solution (0.1 mol/L) titration to the near end point, heated to 50°C in a water bath, continued to slowly titrate until the orange red color disappeared, and corrected the titration result with a blank test. Each 1 ml of cerium sulfate titration solution (0.1 mol/L) corresponds to 19.42mg of C20H24N206.
Last Update：2022-01-01 11:42:42
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Category
Authoritative Data Verified Data
calcium channel blockers.
Last Update：2022-01-01 11:42:42
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Storage
Authoritative Data Verified Data
light shielding, sealed storage.
Last Update：2022-01-01 11:42:42
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Nisoldipine tablet
Authoritative Data Verified Data
This product contains nisoldipine (C20H24N2O6) should be 90.0% to 110.0% of the label.
trait
This product is a film-coated tablet, which shows yellow color after removing the film coating.
identification
In the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the control solution.
examination
- the related substances were protected from light. Take appropriate amount of fine powder of this product, weigh it precisely, add mobile phase, shake to dissolve nisoldipine and quantitatively dilute it into a solution containing about 0.4mg of Nisoldipine per 1ml, filter it, take the continued filtrate as the test solution; Take the reference substance of impurity I and the reference substance of impurity II for precision weighing, add the mobile phase to dissolve and quantitatively dilute to prepare the mixed solution containing about 40ug in each lml, take 3ml with precision, put it in a 100ml measuring flask, add 1ml of human test solution with precision, dilute to scale with mobile phase, shake well, and use as control solution. Nisoldipine was determined according to the method for related substances. If there are chromatographic peaks in the chromatogram of the test solution that are consistent with the retention time of impurity I peak and impurity II peak, the peak area shall be calculated according to the external standard method, and 0.3% of the labeled amount of Nisoldipine shall not be exceeded; the Peak area of other individual impurities shall not be greater than that of Nisoldipine in the control solution (1.0% ) ; The total amount of impurities shall not exceed 1.5%.
- Content uniformity protected from light. Take 1 tablet of this product, grind it in mortar, add a small amount of ethanol to grind it, transfer it to 50ml measuring flask in fractions with ethanol, sonicate Nisoldipine, let it cool, dilute it to scale with ethanol, shake well, filter, and take the continued filtrate as the test solution. Determination of content according to the method under the content determination item, should comply with the provisions (General 0941).
- dissolution rate protected from light. Take this product, according to the dissolution and release determination method (General rule 0931 The first method), with 0.3% sodium dodecyl sulfate solution as the dissolution medium, the rotation speed is 50 rpm, according to the law, after 45 minutes, 10ml of the solution was filtered, and the filtrate was taken as the test solution. About 10mg of the Nisoldipine reference substance was taken, and the solution was placed in a 100ml bottle, add the dissolution medium to dilute to the scale, shake well, take the appropriate amount of children, and quantitatively dilute with the dissolution medium to prepare a solution containing about 5ug per 1 ml as a reference solution. According to the method under the content determination item, the dissolution amount of each tablet was calculated by the peak area according to the external standard method. The limit is 75% of the labeled amount and shall be in accordance with the provisions.
- others shall be in accordance with the relevant provisions under the item of tablets (General rule 0101).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica gel as filler; Methanol-acetonitrile-water (50:15:35) as mobile phase; The detection wavelength was 237nm. The number of theoretical plates shall not be less than 2000 calculated by nisoldine peak, and the separation degree between nisoldine peak and adjacent impurity peaks shall meet the requirements.
- The assay was operated in the dark. Take 20 tablets of this product, precision weighing, fine grinding, precision weighing appropriate amount (about equivalent to Nisoldipine 10mg), put 100ml measuring flask, add appropriate amount of ethanol, ultrasonic dissolution of Nisoldipine, let cool, dilute with ethanol to the scale, shake, filter, take the filtrate as the test solution, take 20 u1, inject into the liquid chromatograph, record the chromatogram; Take the Nisoldipine reference substance, precision weighing, plus ethanol dissolution and quantitative release made per 1 ml containing about 0.lmg solution, the same method for determination. According to the external standard method to calculate the peak area, that is.
category
Same as Nisoldipine.
specification
5mg
storage
light shielding, sealed storage.
Last Update：2022-01-01 11:42:43
Isobutyl Methyl 1,4-Dihydro-2,6-dimethyl-4-(o-nitrophenyl)-3,5-pyridinedicarboxylate - Nisoldipine Capsules
Authoritative Data Verified Data
This product contains nisoldipine (C20H24N206) should be 90.0% ~ 110.0% of the label.
trait
The content of this product is yellow granular powder.
identification
In the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the control solution.
examination
- the related substances were protected from light. Take appropriate amount of fine powder under the content determination item, weigh precisely, add mobile phase, shake to dissolve nisoldipine and quantitatively dilute to make a solution containing about 0.4mg of Nisoldipine per 1 ml, as a test solution; Take the impurity I reference and impurity II reference, precision weighing, plus mobile phase dissolution and quantitative dilution to make a mixed solution containing about 40ug in each lml, take 3ml with precision, put it in a 100ml measuring flask, add 1 ml of human test solution with precision, dilute to scale with mobile phase, shake well, and use as control solution. Nisoldipine was determined according to the method for related substances. If there are chromatographic peaks in the chromatogram of the test solution that are consistent with the retention time of impurity I peak and impurity II peak, the peak area shall be calculated according to the external standard method, and 0.3% of the labeled amount of Nisoldipine shall not be exceeded; the Peak area of other individual impurities shall not be greater than that of Nisoldipine in the control solution (1.0% ) ; The total amount of impurities shall not exceed 1.5%.
- protected from light with uniformity. Take 1 capsule of this product, pour the content into 50ml measuring flask, wash the capsule shell with ethanol, wash the product and put it in the measuring flask, ultrasonic dissolve Nisoldipine, let it cool, dilute with ethanol to the scale, shake, filter, and take the filtrate as the test solution; The content shall be determined according to the method under the content determination item, and shall comply with the regulations (General 0941).
- dissolution rate protected from light. Take this product, according to the dissolution and release determination method (General rule 0931 The first method), with 0.3% sodium dodecyl sulfate solution as the dissolution medium, the rotation speed is 50 rpm, according to the law, after 45 minutes, 10ml of the solution was filtered, and the filtrate was taken as the test solution. Another 10 mg of the Nisoldipine reference product was added to a 100ml measuring flask, and 10ml of ethanol was added, followed by shaking to dissolve the solution, add the dissolution medium to dilute to the scale, shake, take an appropriate amount of precision, and quantitatively dilute with the dissolution medium to prepare a solution containing about 5ug per 1 ml as a reference solution. According to the method under the content determination item, the dissolution amount of each particle was calculated by the peak area according to the external standard method. The limit is 75% of the labeled amount and shall be in accordance with the provisions.
- others should comply with the relevant provisions under the capsule (General 0103).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica gel as filler; Methanol-acetonitrile-water (50:15:35) as mobile phase; The detection wavelength was 237nm. The number of theoretical plates shall not be less than 2000 calculated by nisoldine peak, and the separation degree between nisoldine peak and adjacent impurity peaks shall meet the requirements.
- The assay was operated in the dark. Take 20 capsules of this product, accurately weigh, calculate the average loading, take the content, mix evenly, grind fine, accurately weigh the appropriate amount (about equivalent to 10 mg of Nisoldipine), put it in a 100ml measuring flask, add appropriate amount of ethanol, sonicate to dissolve Nisoldipine, let it cool, dilute to the scale with ethanol, shake well, filter, take the filtrate as the test solution, take 20 u1 with precision, inject into the liquid chromatograph, record the chromatogram; Take another Nisoldipine reference substance, precisely weigh, dissolve and quantitatively dilute with ethanol to make it contain about 0 per 1 ml. lmg solution, the same method for determination. According to the external standard method, the peak area is calculated, that is, the flat reference substance is accurately weighed, dissolved and quantitatively diluted with ethanol to make a solution containing about 0.1 mg per 1 ml, and the same method is used for determination. According to the external standard method to calculate the peak area, that is.
category
Same as Nisoldipine.
specification
5mg
storage
light shielding, sealed storage.
Last Update：2022-01-01 11:42:44
Supplier List
Multiple SpecificationsSpot supply
Product Name: Nisoldipine Visit Supplier Webpage Request for quotationCAS: 63675-72-9
Tel: 18301782025
Email: 3008007409@qq.com
Mobile: 18021002903
QQ: 3008007409
Wechat: 18301782025
Multiple SpecificationsSpot supply
Product Name: Nisoldipine Visit Supplier Webpage Request for quotationCAS: 63675-72-9
Tel: 18301782025
Email: 3008007409@qq.com
Mobile: 18021002903
QQ: 3008007409
Wechat: 18301782025
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