HRID231341

反应详情

EQUATION

反应方程式

HRID 231341 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 15 ml of methylene chloride was dissolved 2.02 g of 4-bromo-2-methoxyimino-3-oxobutyric acid, followed by addition of 2.06 g of phosphorus pentachloride in small portions at 0°-5° C. The mixture was stirred at the same temperature for 5 minutes and, then, at 20°-25° C. for 1 hour, after which it was concentrated under reduced pressure. To the residue was added 20 ml of hexane and the mixture was stirred for a while and allowed to stand. The supernatant was concentrated under reduced pressure to give 2.1 g of 4-bromo-2-methoxyimino-3-oxobutyryl chloride as oil. Yield 96%.

WORKUP

后处理

  1. waitat 20°-25° C. for 1 hour
  2. concentrationafter which it was concentrated under reduced pressure
  3. additionTo the residue was added 20 ml of hexane
  4. stirringthe mixture was stirred for a while
  5. concentrationThe supernatant was concentrated under reduced pressure