HRID1062407

反应详情

EQUATION

反应方程式

HRID 1062407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Acetyl chloride (11.7 ml) was added dropwise to a stirred solution of (R)-2-hydroxy-2-methyl-3,3,3-trifluoropropanoic acid (10 g) (Method 9) in toluene (100 ml) cooled in an ice bath. The mixture was then heated to 80° C. and the suspension dissolved to give a clear solution. After 2 hours the reaction mixture was cooled and then concentrated to give an oil. This oil was then redissolved in DCM (140 ml) and DMF (4 drops) was added followed by oxalyl chloride (6 ml). The solution bubbled vigorously and the reaction mixture was left to stir for 15 hours. The resultant solution of the title compound was used directly without further purification.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. dissolutionthe suspension dissolved
  3. customto give a clear solution
  4. temperatureAfter 2 hours the reaction mixture was cooled
  5. concentrationconcentrated
  6. customto give an oil
  7. customThe solution bubbled vigorously
  8. waitthe reaction mixture was left
  9. customThe resultant solution of the title compound was used directly without further purification