HRID1954056

反应详情

EQUATION

反应方程式

HRID 1954056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3-Isocyano-2,2-dimethyl-succinic acid 1-allyl ester 4-ethyl ester (3.75 g, 15.5 mmol) is dissolved in methanol (100 mL) and the mixture is cooled to 0° C. with an ice bath. To this is added, dropwise, 37% aqueous hydrochloric acid (1.58 g). The reaction is stirred 20 minutes and neutralized with 1 M aqueous sodium hydroxide. The volatiles are removed under vacuum and then the product is extracted into ethyl acetate (2x) and washed with water (2x). The combined organic phases are dried over sodium sulfate and evaporated to give 3-amino-2,2-dimethyl-succinic acid 1-allyl ester 4-ethyl ester as a yellow oil.

WORKUP

后处理

  1. additionTo this is added
  2. customThe volatiles are removed under vacuum
  3. extractionthe product is extracted into ethyl acetate (2x)
  4. washwashed with water (2x)
  5. dry with materialThe combined organic phases are dried over sodium sulfate
  6. customevaporated