HRID232054

反应详情

EQUATION

反应方程式

HRID 232054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 14.1 g (75 mmole) of t-butoxycarbonyl-L-alanine in 135 ml of dry acetonitrile was treated with 12.5 g (77 mmol) of 1,1'-carbonyldiimidazole. After stirring at room temperature for one hour and gas evolution had ceased, the reaction mixture was heated at 60° for one hour cooled to room temperature and treated with 14.2 g (70 mmol) of 3-methyl-1-(phenylmethyl)-3-pyrrolidinemethanamine. The reaction mixture was stirred at room temperature for 18 hours and the solvent was removed in vacuo. The residue was partitioned between ethyl acetate/water and the organic layer was separated, washed with water, dried (MgSO4), and evaporated in vacuo to give 23.9 g of the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated at 60° for one hour
  2. temperaturecooled to room temperature
  3. stirringThe reaction mixture was stirred at room temperature for 18 hours
  4. customthe solvent was removed in vacuo
  5. customThe residue was partitioned between ethyl acetate/water
  6. customthe organic layer was separated
  7. washwashed with water
  8. dry with materialdried (MgSO4)
  9. customevaporated in vacuo