HRID231341
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- waitat 20°-25° C. for 1 hour
- concentrationafter which it was concentrated under reduced pressure
- additionTo the residue was added 20 ml of hexane
- stirringthe mixture was stirred for a while
- concentrationThe supernatant was concentrated under reduced pressure