Name | 1-Amino-4-methylpiperazine |
Synonyms | AMPRZ LABOTEST-BB LT00005082 1-AMINO-4-METHYLPIERAZINE 1-METHYL-4-AMINOPIERAZINE 4-AMINO-1-METHYLPIPERAZINE 1-AMINO-4-METHYLPIPERAZINE 1-Amino-4-methylpiperazine 1-METHYL-4-AMINOPIPERAZINE 4-methylpiperazin-1-ylamine |
CAS | 6928-85-4 |
EINECS | 230-053-7 |
InChI | InChI=1/C5H13N3/c1-7-2-4-8(6)5-3-7/h2-6H2,1H3 |
Molecular Formula | C5H13N3 |
Molar Mass | 115.18 |
Density | 0.957 |
Boling Point | 172-175℃ |
Flash Point | 62℃ |
Water Solubility | miscible |
Refractive Index | 1.4835 |
Physical and Chemical Properties | Character: colorless transparent viscous liquid. boiling point 172-175 ℃ relative density 0.957 refractive index 1.4850 |
Use | Used as a pharmaceutical intermediate for the synthesis of the antibiotic rifampicin |
Hazard Symbols | Xi - Irritant |
Risk Codes | R36/37/38 - Irritating to eyes, respiratory system and skin. |
Safety Description | S24/25 - Avoid contact with skin and eyes. |
UN IDs | 2733 |
colorless transparent viscous liquid. Boiling point 172~175 deg C. Refractive index 4850. Relative density (d40) 0.957. Ignition point: 62 ℃.
low toxicity. Microbial mutation test of a Salmonella typhimurium 10 umol/dish.
piperazine hexahydrate is used as raw material, obtained by methylation, hydrolysis, nitrosation, reduction and other steps. (1) Methylation Dissolve piperazine hexahydrate in formic acid, inhale into a reaction pot, heat up to 90 ℃, add formaldehyde dropwise under stirring for about 1h, finish adding, heat preservation at 90-95 ℃ for 1h, evaporate water and excess raw materials under reduced pressure to obtain methyl formyl piperazine concentrated solution. (2) Hydrolysis Add hydrochloric acid and water to the above concentrated solution, stir and raise the temperature to 105 ℃, and reflow for 2 hours. Distillate under reduced pressure until there is no distillate, discard the distilled acid, cool the residual liquid to 15 ℃, leave it overnight, filter, and the filtrate is methylpiperazine hydrochloride solution. (3) nitrosation will be the hydrolysis step of the filtrate at 30 DEG C dropwise addition of sodium nitrite solution, after the addition, heat preservation reaction for 30min, methyl nitropiperazine generation solution. (4) Reduction Add glacial acetic acid into the nitrosation generating solution, cool it, gradually add zinc powder at 30-40 ℃, finish it, keep the temperature at 30-40 ℃ for 1.5h, cool it to about 15 ℃, leave it overnight, and filter it. Add this reduction filtrate to an alkalizing pot that has been prepared with liquid alkali and cooled to below 10°C, fully cool and send it to an extraction pot, add chloroform for extraction in 3 times, merge the chloroform extract, and perform normal pressure Distillation to recover chloroform, transfer to a rectification pot when the liquid temperature is 85 ℃, first distill the liquid temperature is 135 ℃, and then perform vacuum distillation, the fraction collected at 120 ℃(5.33-8.0kPa) is 1-amino-4-methylpiperazine. The total yield of the above four steps is about 30%. Raw material consumption quota: piperazine hexahydrate (95%)1148.1kg/t, formic acid (85%)2266.2kg/t, formaldehyde (37%)1130.8kg/t, zinc powder (90%)1900.2kg/t, glacial acetic acid 3759.4kg/t, concentrated hydrochloric acid 4046.5kg/t, sodium nitrite 937.6kg/t.
storage conditions | Keep in dark place,Inert atmosphere,Room temperature |
solubility | water: soluble |
acidity coefficient (pKa) | 7? -. 0.42(Predicted) |
morphology | Viscous Solution |
color | Clear |
water solubility | miscible |
sensitivity | Air & Light Sensitive |
BRN | 103334 |
InChIKey | RJWLLQWLBMJCFD-UHFFFAOYSA-N |
NIST chemical information | 1-Amino-4-methylpiperazine(6928-85-4) |
WGK Germany | 3 |
HazardClass | 3 |
PackingGroup | III |
customs code | 29335995 |