HRID1857058

反应详情

EQUATION

反应方程式

HRID 1857058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Then potassium carbonate (66.96 g, 0.485 mol) was added to a mixture of (R)-4-acetoxymethyl-2,2-dimethyl-1,3-dioxolane (56.32 g, 0.323 mol) and methanol (400 ml) and resulting mixture was stirred for 8 hours at 25° C. After completion of the reaction the salt was filtered off and the filtrate was condensed in vacuo. Water was added to the residue and the mixture was extracted with methylene chloride. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and condensed in vacuo. The crude product was distilled to give 38.27 g of (S)-2,2-dimethyl-1,3-dioxolane-4-methanol (yield 87%, b.p. 65° C. at 3 mmHg, optical purity 97.5% e.e., specific rotation [α]D20+ 10.87°(c=1,MeOH)).

WORKUP

后处理

  1. customresulting mixture
  2. customAfter completion of the reaction the salt
  3. filtrationwas filtered off
  4. customcondensed in vacuo
  5. extractionthe mixture was extracted with methylene chloride
  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