HRID406963

反应详情

EQUATION

反应方程式

HRID 406963 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a round bottom flask, (0.9 g) 3-hydroxy-2-(hydroxymethyl)-2-methylpropanoic acid and (9.8 mg) p-toluene sulfonic acid and 2 ml toluene was taken. The reaction mixture was stirred at room temperature and subsequently 2 g (1 equiv) bis-(4-chlorophenyl)-dimethoxymethane [IIa4] diluted with 5 ml toluene was added through droping funnel. The reaction mixture was heated at reflux temperature and the water was removed azeotropically under Dean Stark. Continuous removal and addition of toluene was done up to 2 hrs. Then the reaction mixture was cooled at room temperature to obtain off white solid. It was filtered and washed with toluene and then water.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux temperature
  4. customthe water was removed azeotropically under Dean Stark
  5. customContinuous removal and addition of toluene
  6. temperatureThen the reaction mixture was cooled at room temperature
  7. customto obtain off white solid
  8. filtrationIt was filtered
  9. washwashed with toluene