HRID376734

反应详情

EQUATION

反应方程式

HRID 376734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

The title compound was prepared as described in U.S. Pat. Nos. 2,590,632 and 2,620,343. At 10° C., 30 g of benzidine sulfate was added, in portions, to 100 ml of fuming sulfuric acid. After the addition, the reaction was maintained at 70° C. for 18 hours, cooled and poured into 250 g of cracked ice. The beige solid was collected, washed with water and saturated sodium bicarbonate yielding a yellow solid. The yellow solid was stirred with bicarbonate solution 2×, collected, washed with large volumes of water, and dried in vacuo to give 22.66 g (87%) of the desired product.

WORKUP

后处理

  1. customThe title compound was prepared
  2. additionAfter the addition
  3. temperaturecooled
  4. customThe beige solid was collected
  5. washwashed with water and saturated sodium bicarbonate yielding a yellow solid
  6. customcollected
  7. washwashed with large volumes of water
  8. customdried in vacuo