HRID1106600

反应详情

EQUATION

反应方程式

HRID 1106600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a R.T. solution of 2-chloroacetic acid 2-methyl-1-(4-(methylsulfonyl)phenyl)propan-1-one ester (954 mg, 3 mmol, example 25) in acetonitrile (15 mL) was added 3,5-dichloro-2-pyridone (656 mg, 4.0 mmol) followed by DBU (2.28 g, 15 mmol) and the mixture was slowly warmed up to gentle reflux for 2 hours. The mixture was cooled to 25° C. the volatiles were removed in vacuo. The residue was purified on silica gel chromatography (1/1, EtOAc/Hexanes then 100% EtOAc)) to provide the title compound.

WORKUP

后处理

  1. temperaturethe mixture was slowly warmed up
  2. temperatureto gentle reflux for 2 hours
  3. customwere removed in vacuo
  4. customThe residue was purified on silica gel chromatography (1/1, EtOAc/Hexanes