HRID217155

反应详情

EQUATION

反应方程式

HRID 217155 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) at ambient temperature giving a white suspension. Methylthioacetic acid (1.0 g) was dissolved in DMF (5 ml) then added to the amine followed by HOBT (1.27 g) and finally EDC (1.806 g). The white suspension was stirred at room temperature for 6 hours and stored overnight. Water was added and the aqueous phase was extracted with diethyl ether. The organic phases were combined, successively washed with water and dried over magnesium sulphate, filtered and evaporated under reduced pressure 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 overnight
  3. extractionthe aqueous phase was extracted with diethyl ether
  4. washsuccessively washed with water
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure