HRID45307

反应详情

EQUATION

反应方程式

HRID 45307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixed solvent comprising 6 ml of methanol and 5 ml of water, there was suspended 1.56 g of N-(2-fluoroethyl)-N-methylmethoxyoxalylamide, then 3.2 g of a 15% aqueous solution of sodium hydroxide was dropwise added, with ice-cooling, to the suspension and then the mixture was stirred for one hour. Concentrated hydrochloric acid was added to the reaction system, the mixture was then extracted with ethyl acetate, the organic phase thus separated was washed with water, dried over magnesium sulfate and then the ethyl acetate was distilled off from the organic phase to thus give, as the target product, 0.94 g (yield: 66%, a solid product) of N-(2-fluoroethyl)-N-methylaminooxamic acid.

WORKUP

后处理

  1. temperaturecooling, to the suspension
  2. extractionthe mixture was then extracted with ethyl acetate
  3. customthe organic phase thus separated
  4. washwas washed with water
  5. dry with materialdried over magnesium sulfate
  6. distillationthe ethyl acetate was distilled off from the organic phase
  7. customto thus give, as the target product, 0.94 g (yield: 66%