HRID2309181

反应详情

EQUATION

反应方程式

HRID 2309181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To a solution of tert-butyl isocyanate (0.991 g) in methylene chloride (8 ml) was added dropwise to a mixture of N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (1.012 g) in methylene chloride (40 ml) under ice bath cooling. The mixture was stirred for an hour at about 5° C. The reaction mixture was evaporated to dryness, and then the residue was dissolved in ethyl acetate (50 ml). The solution was washed with water (40 ml), dried over magnesium sulfate and evaporated to dryness. The crude residue was washed with ether and dried to give N-[(tert-butylcarbamoyl)amino]-1,2,3,6-tetrahydropyridine (0.50 g).

WORKUP

后处理

  1. temperaturecooling
  2. customThe reaction mixture was evaporated to dryness
  3. dissolutionthe residue was dissolved in ethyl acetate (50 ml)
  4. washThe solution was washed with water (40 ml)
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness
  7. washThe crude residue was washed with ether
  8. customdried