HRID251392
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 94 °C
PROCEDURE
实验过程
4-Amino-2-methyl-10H-thieno-[2,3-b][1,5]benzodiazepine (5 g, 0.02 mol), N-methylpiperazine (12.5 mL, 2.5 vol) and ethanol (15 mL, 3 vol) were charged into a three-necked round bottom flask equipped with a reflux condenser, overhead stirrer, and thermometer. The reaction mixture was slowly heated to reflux (94° C.) under a nitrogen atmosphere and kept at this temperature overnight. The reaction mixture was cooled to below 50° C. and water (10 mL, 2 vol) was added to precipitate out the solid, which was isolated by filtration. The light yellow solid was washed twice with water (5 mL) and dried to furnish pure olanzapine in 72% yield (4.2 g).
WORKUP
后处理
- customequipped with a reflux condenser, overhead stirrer
- temperatureThe reaction mixture was slowly heated
- customkept at this temperature overnight
- temperatureThe reaction mixture was cooled to below 50° C.
- customto precipitate out the solid
- customwhich was isolated by filtration
- washThe light yellow solid was washed twice with water (5 mL)
- customdried