HRID411514

反应详情

EQUATION

反应方程式

HRID 411514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

A mixture of 2,3-indolinedione (5 g, 0.03 mole), 3′,4′-difluoroacetophenone (5 g, 0.03 mole) and potassium hydroxide (3 g, 0.05 mole) in 1,4-dioxane (50 mL) is heated at 105° C. for 48 hours. The reaction solution is then cooled to room temperature and concentrated under reduced pressure. The residue is treated with EtOAc and extracted with water. The pH of the aqueous layer is adjusted to 5-6 with 1N HCl, the resulting solid is collected by vacuum filtration, washed with water, and dried to give the titled compound (450 mg) as a yellow solid.

WORKUP

后处理

  1. temperatureThe reaction solution is then cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue is treated with EtOAc
  4. extractionextracted with water
  5. filtrationthe resulting solid is collected by vacuum filtration
  6. washwashed with water
  7. customdried