HRID251392

反应详情

EQUATION

反应方程式

HRID 251392 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customequipped with a reflux condenser, overhead stirrer
  2. temperatureThe reaction mixture was slowly heated
  3. customkept at this temperature overnight
  4. temperatureThe reaction mixture was cooled to below 50° C.
  5. customto precipitate out the solid
  6. customwhich was isolated by filtration
  7. washThe light yellow solid was washed twice with water (5 mL)
  8. customdried