HRID448258

反应详情

EQUATION

反应方程式

HRID 448258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

62 g (0.23 mol) of N-(tert-butoxycarbonyl)-N-(2-cyanoethyl)-2-methylalanine were dissolved in 350 ml of DMF and 50 g of KHCO3 were added. Few minutes after, 30 ml of methyl iodide (MeI) were dropped and the mixture was stirred at room temperature for 6 hours. Then a further 15 ml of MeI were added. The mixture was left at room temperature overnight. After dilution with 1.5 l of water, the solution was extracted with ethyl acetate (3 times). The organic phases were washed with a small amount of water, dried over sodium sulfate, evaporated and dried at the mechanical pump. 60.5 g (97%) of methyl N-(tert-butoxycarbonyl)-N-(2-cyanoethyl)-2-methylalaninate were thus obtained.

WORKUP

后处理

  1. waitThe mixture was left at room temperature overnight
  2. extractionAfter dilution with 1.5 l of water, the solution was extracted with ethyl acetate (3 times)
  3. washThe organic phases were washed with a small amount of water
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customdried at the mechanical pump