HRID563887

反应详情

EQUATION

反应方程式

HRID 563887 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Triethylamine (1.84 ml) was added to a stirred solution of 4-amino-4-methyl-pent-2-yne hydrochloride (1.278 g) in DMF (5 ml) giving a white suspension. Methylthioacetic acid (1.0 g) in DMF (5 ml) was then added to the amine followed by the HOBT (1.27 g) and finally EDC (1.806 g). The white suspension was stirred at ambient temperature for 6 hours, and stored for 18 hours. Water was added and the aqueous phase was extracted with diethyl ether. The organic phases were combined, washed with water and dried over magnesium sulphate then filtered and evaporated to give 2-(methylthio)-N-(2-methylpent-3-yn-2-yl) acetamide as a yellow orange solid (1.9 g).

WORKUP

后处理

  1. customgiving a white suspension
  2. waitstored for 18 hours
  3. extractionthe aqueous phase was extracted with diethyl ether
  4. washwashed with water
  5. dry with materialdried over magnesium sulphate
  6. filtrationthen filtered
  7. customevaporated