HRID398993

反应详情

EQUATION

反应方程式

HRID 398993 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

A solution of 2 g of sodium nitrite in 60 ml of water was added at 0° C. to a suspension at 0° C. of 3.2 g of the product of Step A in 100 ml of concentrated hydrochloric acid, and the mixture was stirred for 90 minutes at 0° C., then for one hour at 100° C. The reaction medium was poured into 100 ml of ice-cooled water, separated and washed with ice-cooled water. The moist product was taken up in 100 ml of water and alkalized with concentrated ammonium hydroxide. After separation, the residue was washed with water and dried at 70° C. under reduced pressure to obtain 1.47 g of the expected product melting at 180° C.

WORKUP

后处理

  1. waitfor one hour at 100° C
  2. customseparated
  3. washwashed with ice-
  4. temperaturecooled water
  5. customAfter separation
  6. washthe residue was washed with water
  7. customdried at 70° C. under reduced pressure