HRID750638

反应详情

EQUATION

反应方程式

HRID 750638 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

NaBH4 (566 mg, 14.91 mmol) was added to a stirring solution of 2-methyl-isoindole-1,3-dione (2.0 g, 12.42 mmol) in methanol (20 mL) at 0° C. Stirring at 0° C. was maintained for 1 hour, then the reaction was warmed to room temperature. Additional NaBH4 (566 mg, 14.91 mmol) was added in order to push the reaction to completion. The reaction was then quenched with acetic acid (5 mL) and partitioned between water and dichloromethane. The organic layer was washed several times with water and concentrated under vacuum to give 659 mg of the sub-title compound as a white solid. MS: ESI (positive): 164 (M+H).

WORKUP

后处理

  1. temperaturewas maintained for 1 hour
  2. temperaturethe reaction was warmed to room temperature
  3. customthe reaction to completion
  4. customThe reaction was then quenched with acetic acid (5 mL)
  5. custompartitioned between water and dichloromethane
  6. washThe organic layer was washed several times with water
  7. concentrationconcentrated under vacuum