HRID241594

反应详情

EQUATION

反应方程式

HRID 241594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

2-chloro-N-(3-methoxyphenyl)acetamide (3.1 g, 16 mmol) and anhydrous AlCl3 powder (4.4 g, 32 mmol) is heated and stirred at 120° C. for 10 minutes and exhibit a melting state. The temperature is elevated gradually to 240° C. in 40 minutes and then stirred 5 minutes. The reaction is allowed to cool to obtain a brown powder. The solid powder is poured into a mixture of 100 g of crushed ice and 50 ml of concentrated hydrochloric acid. The mixture is stirred for 10 minutes and then reflux for 10 minutes, and allowed to cool to precipitate a light yellow powder, which is filtered out and recrystallized in water to obtain 1.5 g of 6-hydroxy-indoline-2-one, with a yield of 62%.

WORKUP

后处理

  1. waitThe temperature is elevated gradually to 240° C. in 40 minutes
  2. stirringstirred 5 minutes
  3. temperatureto cool
  4. customto obtain a brown powder
  5. stirringThe mixture is stirred for 10 minutes
  6. temperaturereflux for 10 minutes
  7. temperatureto cool
  8. customto precipitate a light yellow powder, which
  9. filtrationis filtered out
  10. customrecrystallized in water