HRID383484

反应详情

EQUATION

反应方程式

HRID 383484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-hydroxy-5, 5-dimethyl-5H-furan-2-one (2.1 g, 16.4 mmol) in DCE (40 mL) and DMF (1.5 mL) at 0° C. was added dropwise oxalyl bromide (3.0 mL, 32 mmol, 2 equiv). The mixture was stirred at room temperature for 4-5 h, and then put in an ice bath. Ice water (100 mL) was added slowly. The mixture was extracted with CH2Cl2 (100 mL). The organic phase was washed with 10% NaHCO3 and again with water, dried over sodium sulfate and evaporated to give the title compound 2.7 g (86% yield).

WORKUP

后处理

  1. customput in an ice bath
  2. extractionThe mixture was extracted with CH2Cl2 (100 mL)
  3. washThe organic phase was washed with 10% NaHCO3 and again with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated