HRID236987

反应详情

EQUATION

反应方程式

HRID 236987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.98 gm. (0.39 mole) of sodium in 180 ml. of anhydrous ethanol is added to a solution of 26.8 gm. (0.386 mole) of hydroxylamine hydrochloride in 270 ml. of hot ethanol. The precipitate is removed by filtration. To the stirred filtrate is added 34.2 gm. (0.26 mole) of ethyl 2-thiooxamate. The yellow solution is allowed to stand overnight. The solution is evaporated to dryness in vacuo and the residue recrystallized from diethyl ether. There is obtained 21.2 g. (68%) of a yellow solid melting at 99°-101° C.

WORKUP

后处理

  1. customThe precipitate is removed by filtration
  2. additionTo the stirred filtrate is added 34.2 gm
  3. customThe solution is evaporated to dryness in vacuo
  4. customthe residue recrystallized from diethyl ether
  5. customThere is obtained 21.2 g