HRID656314

反应详情

EQUATION

反应方程式

HRID 656314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a 1000 ml round-bottom flask fitted with a thermometer, a nitrogen-introducing tube, and a stirrer were added 132.2 g (1.0 mol) of 2,2-dimethyl-1,3-dioxolane-4-methanol, 231.4 g (1.2 mol) of a 28% methanol solution of sodium methoxide, and 500 ml of toluene. With introducing nitrogen thereinto, the toluene was refluxed under reduced pressure for 1 hour to remove the methanol by distillation. With maintaining the solution at 80° C., 126.6 g (1.0 mol) of benzyl chloride was added dropwise over a period of 2 hours using a dropping funnel, followed by further 2 hours of the reaction. The reaction solution was subjected to solvent removal and purification by distillation (b.p. 93-95° C./266 Pa) to obtain 4-(benzyloxymethyl)-2,2-dimethyl-1,3-dioxolane.

WORKUP

后处理

  1. customTo a 1000 ml round-bottom flask fitted with a thermometer
  2. additiona nitrogen-introducing tube, and a stirrer
  3. customto remove the methanol
  4. distillationby distillation
  5. customfollowed by further 2 hours of the reaction
  6. customThe reaction solution was subjected to solvent removal and purification by distillation (b.p. 93-95° C./266 Pa)