HRID1962316

反应详情

EQUATION

反应方程式

HRID 1962316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-tert-butyl-5-(methoxycarbonyl)benzoic acid (9.18 g, 38.9 mmol, prepared by the method of Carter et. al., WO2005021500A1), thionyl chloride (75 mL) and 1 drop of DMF in toluene (200 mL) was heated at reflux for 2 h, cooled and concentrated. The residue was azeotroped with toluene (3×50 mL) and dried under high vacuum to give the title compound as an off-white waxy solid (9.9 g, quantitative yield).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 h
  3. temperaturecooled
  4. concentrationconcentrated
  5. customThe residue was azeotroped with toluene (3×50 mL)
  6. customdried under high vacuum