HRID236226

反应详情

EQUATION

反应方程式

HRID 236226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.0 g of 2-amino-3-cyano-4-(1,1-dimethylethyl)thiophene and 4.0 g of 2-methyl-4-chlorobutyryl chloride dissolved with 100 ml benzene was refluxed for about 72 hours. The solvent was evaporated under reduced pressure and the residue was chromatographed while eluting with a 90/10 mixture of Skellysolve B/ethyl acetate. Fractions containing the major component were combined and the solvent was evaporated therefrom to afford 3.75 g of 4-chloro-N-[3-cyano-4-(1,1-dimethylethyl)-2-thienyl]-2-methylbutanamide. mp=115°-116° C. Yield 57%.

WORKUP

后处理

  1. temperaturewas refluxed for about 72 hours
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was chromatographed
  4. washwhile eluting with a 90/10 mixture of Skellysolve B/ethyl acetate
  5. additionFractions containing the major component
  6. customthe solvent was evaporated