HRID236226
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for about 72 hours
- customThe solvent was evaporated under reduced pressure
- customthe residue was chromatographed
- washwhile eluting with a 90/10 mixture of Skellysolve B/ethyl acetate
- additionFractions containing the major component
- customthe solvent was evaporated