HRID2083717

反应详情

EQUATION

反应方程式

HRID 2083717 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(3-Methoxycarbonyl-2-methylpropanoyl)-L-proline (2.4 g.) is dissolved in a mixture of dichloromethane (50 ml.) and triethylamine (1.4 ml.). The solution is chilled in an ice water bath and isobutylchloroformate (1.36 g.) is added while the mixture is stirred. After 10 minutes ammonia (gas) is bubbled through the solution, still in the ice bath, for 15 minutes. The reaction mixture is stirred for one hour at room temperature, diluted with methylene chloride (100 ml.) and washed with water, 0.1 N hydrochloric acid, water, and dried over magnesium sulfate. The solvent is removed in vacuo to yield 1-(3-methoxycarbonyl-2-methylpropanoyl)-L-prolineamide.

WORKUP

后处理

  1. temperatureThe solution is chilled in an ice water bath
  2. customAfter 10 minutes ammonia (gas) is bubbled through the solution, still in the ice bath, for 15 minutes
  3. stirringThe reaction mixture is stirred for one hour at room temperature
  4. additiondiluted with methylene chloride (100 ml.)
  5. washwashed with water, 0.1 N hydrochloric acid, water
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent is removed in vacuo