66722-57-4
[[4-[[2-(1-Methylethoxy)ethoxy]methyl]phenoxy]methyl]oxirane
CAS: 66722-57-4
Molecular Formula: C15H22O4
66722-57-4 - Names and Identifiers
66722-57-4 - Physico-chemical Properties
| Molecular Formula | C15H22O4 |
| Molar Mass | 266.33 |
| Density | 1.084±0.06 g/cm3(Predicted) |
| Boling Point | 362.6±22.0 °C(Predicted) |
| Flash Point | 118.2°C |
| Solubility | Chloroform (Slightly), Methanol (Sparingly) |
| Vapor Presure | 3.99E-05mmHg at 25°C |
| Appearance | Oil |
| Color | Colourless |
| Storage Condition | Refrigerator |
| Refractive Index | 1.508 |
66722-57-4 - Preparation solution concentration reference
| 1mg | 5mg | 10mg | |
|---|---|---|---|
| 1 mM | 3.755 ml | 18.774 ml | 37.547 ml |
| 5 mM | 0.751 ml | 3.755 ml | 7.509 ml |
| 10 mM | 0.375 ml | 1.877 ml | 3.755 ml |
| 5 mM | 0.075 ml | 0.375 ml | 0.751 ml |
Last Update：2024-01-02 23:10:35
66722-57-4 - Reference Information
| Introduction | [[4-[2-(1-methylethoxy)] ethoxy] methyl] phenoxy] methyl] oxirane is an epoxy impurity of the selective β1-adrenergic receptor blocker Bisoprolol. [[4-[2-(1-methylethoxy) ethoxy] methyl] phenoxy] methyl] oxirane the intermediate 4-hydroxybenzyl alcohol can be prepared from 4-hydroxybenzaldehyde, further, 4-[(2-isopropoxyethoxy) methyl]-phenol is prepared by reaction with 2-isopropoxyethanol and finally with epichlorohydrin. |
| preparation | 1) preparation of 4-hydroxybenzyl alcohol in a 250L reactor, 8.33kg of sodium hydroxide was dissolved in water, and 25.0kg of 4-hydroxybenzaldehyde was added, the reaction mixture was stirred to obtain a clear solution, the reaction mixture was cooled to 15 °c, A 3.0kg solution of sodium borohydride in 15L of water at 15-20 °c was added over a period of about 3 hours. The reaction mixture was further stirred for 3 hours, and a 1.0 charcoal slurry prepared in water was added to the reaction mixture, stirred for an additional 30 minutes, and filtered over a Celite bed. The reaction mixture was collected in a 400L reactor and cooled to 0-5°C; A dilute solution of acetic acid (20kg of a 20kg solution diluted with 20L of water) was added within 3-5 hours at 0-5°C slowly added to the reaction mixture, the isolated product was filtered and washed with 40L of water, spin-dried and dried under vacuum to obtain 21-23kg of 4-hydroxybenzyl alcohol in a yield of 21-23kg. 2) preparation of 4-[(2-isopropoxyethoxy) methyl]-phenol in a 400 liter reactor, 280 liter of 2-isopropoxyethanol was added and cooled to 0 °c. Will be a batch Amberlyst-15(22.5) The resin was added thereto, 4-hydroxybenzyl alcohol (22.5) was added in small portions of 2kg per batch over a period of about 5 hours at 0-5°C, and the reaction mixture was stirred at 0-5°C for 2 hours, the temperature was raised to 15-20 °c and held for 10 hours. The resin was filtered off and washed with 2-isopropoxyethanol, and the reaction mixture was collected in a Amberlyst-15 L vessel and basified with of potassium carbonate. The potassium carbonate was filtered and the reaction mixture was distilled to give 36-38kg of 4-[(2-isopropoxyethoxy) methyl]-phenol in a yield of 36-38kg. 3) preparation of [[4-[[2-(1-methylethoxy) ethoxy] methyl] phenoxy] methyl] oxirane reaction of an aqueous solution of methyl]-phenol sodium salt with 90kg of Epichlorohydrin at 60-65°C for 1 hour, The reaction mixture was then extracted twice with 90L of toluene, the toluene extract was stirred with 7.2kg of solid sodium hydroxide, the reaction mixture was washed three times with water, and the toluene layer was distilled. After removal of the solvent, [[4-[[2-(1-methylethoxy) ethoxy] methyl] phenoxy] methyl] oxirane is obtained as an oil, the product was further purified by high vacuum distillation at 0.5mm at 160-200 °c to give purified [[4-[[2-(1-methylethoxy) ethoxy] methyl] phenoxy] methyl] oxirane. |
Last Update：2024-04-10 22:29:15
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Product Name: [[4-[[2-(1-Methylethoxy)ethoxy]methyl]phenoxy]methyl]oxirane Visit Supplier Webpage Request for quotation
CAS: 66722-57-4
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