HRID1091027

反应详情

EQUATION

反应方程式

HRID 1091027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 9.3 g of the above benzamide and 200 ml of methanolic ammonia was added dropwise, 10 ml of 30% hydrogen peroxide over 3 minutes. An exotherm required cooling in an ice bath. A 15 ml portion of 30% hydrogen peroxide was added, the mixture was stirred 48 hours, the solid collected, and mixed with 100 ml of hot water. This solid was collected, mixed with 400 ml of hot acetonitrile and filtered. The filtrate was chilled, giving 2.3 g of the desired product as off-white crystals, mp 211°-213° C.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureAn exotherm required cooling in an ice bath
  3. customthe solid collected
  4. additionmixed with 100 ml of hot water
  5. customThis solid was collected
  6. additionmixed with 400 ml of hot acetonitrile
  7. filtrationfiltered
  8. temperatureThe filtrate was chilled