HRID2287347

反应详情

EQUATION

反应方程式

HRID 2287347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-bromo-6-chlorobenzoic acid chloride (0.5 mmol) in dichloromethane (5 ml) was added dropwise to a solution of 2,3-dihydro-4-pyridinone (5.1 mmol, 495 mg) and triethylamine (1.2 ml) in dichloromethane (20 ml). After stirring for 30 minutes, the solution was diluted with water, separated, the aqueous extract further extracted with dichloromethane, the combined organic extracts combined and washed with brine, dried over sodium sulphate and evaporated. The residue was purified by flash column chromatography on silica eluting with 30% ethyl acetate in hexane to yield the title compound as a pale yellow oil (629 mg). MS (+CI) m /z 316 [M+H]+.

WORKUP

后处理

  1. customseparated
  2. extractionthe aqueous extract further
  3. extractionextracted with dichloromethane
  4. washwashed with brine
  5. dry with materialdried over sodium sulphate
  6. customevaporated
  7. customThe residue was purified by flash column chromatography on silica eluting with 30% ethyl acetate in hexane