HRID2112488

反应详情

EQUATION

反应方程式

HRID 2112488 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 0.10 g (0.00033 mole) of 5-(2-chlorophenyl)-7,8-difluoro-1,3-dihydro-2H-1,4-benzodiazepin-2-one (Imm), 2 mL of methanol and 0.03 g of sodium hydride was heated at 100° C. for 40 minutes using microwave heating in a sealed reaction vessel. The mixture was then cooled. diluted with ethyl acetate and washed successively with water and then brine. The mixture was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give 0.103 g of 5-(2-chlorophenyl)-1,3-dihydro-7-fluoro-8-methoxy-2H-1,4-benzodiazepin-2-one (Ia) as a white solid. MH+/Z=319.

WORKUP

后处理

  1. temperatureusing microwave heating in a sealed reaction vessel
  2. temperatureThe mixture was then cooled
  3. washwashed successively with water
  4. dry with materialThe mixture was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure