Midazolam synthesis
- Product Name:Midazolam
- CAS Number:59467-64-0
- Molecular formula:C16H15ClFN3
- Molecular Weight:303.76
Yield:59467-64-0 2.201kg
Reaction Conditions:
Stage #1:2-amino-5-chloro-2'-fluorobenzophenone;epichlorohydrin with ammoniaLarge scale;
Stage #2: with phosphorus pentoxide at 70 - 80; for 5 h;Large scale;
Steps:
VII
After the reaction vessel are then added to 2500g substance A, after 2- (chloromethyl) oxirane 920g Stir slowly leads to ammonia 400g, all the ammonia into the reaction vessel, the reaction was stirred for 1-2 hours, after the reaction until smooth, stirring slowly added 200g of phosphorus pentoxide, when all the mixing of raw materials, the reaction was heated to 70-80 five hours. After cooling, water was added 1000g, adjust pH to alkaline three times with 8000g of n-hexane reaction was extracted, liquid separation and the organic layer was evaporated under reduced pressure low viscosity, using hexane: ethanol = 5: 1 solvent the above reaction was recrystallized and vacuum dried to obtain 2201g of product.By HPLC> 99%.
References:
Wangzhixun;Wang, zhixun CN104447687, 2016, B Location in patent:Paragraph 0089-0093
