HRID607140

反应详情

EQUATION

反应方程式

HRID 607140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product of Example 5D (212.7 mg, 1.496 mmol) in anhydrous ethanol (5 mL) was treated with Meldrum's acid (237 mg, 1.645 mmol) and triethylorthoformate (0.25 mL, 1.496 mmol) at room temperature, and the reaction was heated in a preheated 100° oil bath. After 15 minutes, the reaction was cooled to room temperature and the solvent removed by rotary evaporation under vacuum. Purification by silica gel flash chromatography with a gradient of 10% to 20% ethyl acetate/methylene chloride afforded the title compound as an off-white solid (240 mg, 0.8099 mmol, 54%).

WORKUP

后处理

  1. temperaturethe reaction was heated in a preheated 100° oil bath
  2. customthe solvent removed by rotary evaporation under vacuum
  3. customPurification by silica gel flash chromatography with a gradient of 10% to 20% ethyl acetate/methylene chloride