HRID1477981

反应详情

EQUATION

反应方程式

HRID 1477981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a suspension of LAH (22.80 g, 600 mmol) in THF (600 mL) at 0° C. was added tetrahydrophthalimide (39.45 g, 260.9 mmol) portionwise. After addition, the reaction mixture was stirred at 60° C. for 18 h, then cooled down to 0° C. and quenched carefully with water (25 mL), followed by 15% KOH aqueous solution (25 mL) and another 75 mL of water. The resulting mixture was stirred at rt for 1 h and filtered through a pad of Celite, then washed with DCM (500 mL). The filtrate was concentrated in vacuo to give isoindole as yellow oil, which was used in the next step without purification.

WORKUP

后处理

  1. additionAfter addition
  2. temperaturecooled down to 0° C.
  3. customquenched carefully with water (25 mL)
  4. stirringThe resulting mixture was stirred at rt for 1 h
  5. filtrationfiltered through a pad of Celite
  6. washwashed with DCM (500 mL)
  7. concentrationThe filtrate was concentrated in vacuo