HRID1857057

反应详情

EQUATION

反应方程式

HRID 1857057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Sodium bromide (57.93 g, 0.563 mol) and sodium acetate (46.18 g, 0.563 mol) were added to a mixture of (R)-4-chloromethyl-2,2-dimethyl-1,3-dioxolane (84.76 g, 0.563 mol) prepared by the same manner as Example 3 and N,N-dimethylformamide (800 ml) and the resulting mixture was stirred for 15 hours at 150° C. After cooling the salt was filtered off and N,N-dimethylformamide was removed in vacuo and water was added to the residue and extracted with toluene. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and condensed in vacuo. The crude product was distilled to give 60.81 g of (R)-4-acetoxymethyl-2,2-dimethyl-1,3-dioxolane (yield 62%, b.p. 78° C. at 10 mmHg).

WORKUP

后处理

  1. temperatureAfter cooling the salt
  2. filtrationwas filtered off
  3. customN,N-dimethylformamide was removed in vacuo and water
  4. additionwas added to the residue
  5. extractionextracted with toluene
  6. washThe extract was washed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate and condensed in vacuo
  8. distillationThe crude product was distilled