HRID267232

反应详情

EQUATION

反应方程式

HRID 267232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 77 g. (0.5 mole) of 5-chloroindoline, 80 ml. of concentrated hydrochloride acid and 500 ml. of crushed ice was stirred while a solution of 35 g. of sodium nitrite in 100 ml. of water was added over five minutes. The temperature was kept between 10°C. to 15°C. by addition of ice. The mixture was stirred for 1 hour and then filtered. Recrystallization of the product from benzene-isooctane gave 57 g. (68%) of product which melted at 120°-122°C.

WORKUP

后处理

  1. additionA mixture of 77 g
  2. additionThe temperature was kept between 10°C. to 15°C. by addition of ice
  3. stirringThe mixture was stirred for 1 hour
  4. filtrationfiltered
  5. customRecrystallization of the product from benzene-isooctane
  6. customgave 57 g