HRID1247870

反应详情

EQUATION

反应方程式

HRID 1247870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 6.23 g t-butylhydrazine hydrochloride (0.050 moles) in 50 mL tetrahydrofuran was degassed, then stirred under nitrogen as, first, one equivalent of powdered potassium hydroxide and then, dropwise, 2.85 g methyl isocyanate in 25 mL tetrahydrofuran were added. The solution was stirred overnight. The mixture was filtered to remove the residual solid impurity which was washed several times with tetrahydrofuran. The combined filtrates were evaporated to yield a white product which was taken up in chloroform and dried. Removal of the solvent yielded 5.80 g (79.9%) white crystalline N-methyl-1-t-butylhydrazinecarboxamide (m.p. 127°-9° C.). This structure was confirmed by NMR analysis.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customto remove the residual solid impurity which
  3. washwas washed several times with tetrahydrofuran
  4. customThe combined filtrates were evaporated
  5. customto yield a white product which
  6. customdried
  7. customRemoval of the solvent