HRID607591

反应详情

EQUATION

反应方程式

HRID 607591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 4-(oxoacetyl)benzoate (13.5 g, 0.0702 mol), ethyl orthoformate (29 mL, 0.18 mol), p-toluenesulfonic acid monohydrate (0.7 g) in toluene (150 mL) was heated under reflux for 2 h. After cooling, the solvent was removed under reduced pressure. The crude material was flash chromatographed on a silica gel column to afford the desired product (15.4 g, 82%). Analytical LCMS: (M+Na)+=289.0.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 h
  3. temperatureAfter cooling
  4. customthe solvent was removed under reduced pressure
  5. customchromatographed on a silica gel column