HRID1374926

反应详情

EQUATION

反应方程式

HRID 1374926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

The neat mixture of S (−) 2-chloro-1-phenylethanol (2.78 g., 17.8 mmol) and 4,5-dimethylthiazole (2 g., 17.7 mmol) were heated with stirring at 135° C. for 25 hrs. It was cooled to room temperature and water (30 mL) was added to the reaction mixture with stirring. The solution was extracted with ether (30 mL). The ether extract was again extracted with water (30 mL). The combined water layer was evaporated to dryness and the residue was crystallized with a mixture of acetonitrile and methyl tert-butyl ether. Yield: 0.63 g. (7.7%); mp. 189–190° C.; [α]D25−51.765 (Water, c=1.7732).

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureIt was cooled to room temperature
  3. stirringwith stirring
  4. extractionThe solution was extracted with ether (30 mL)
  5. extractionThe ether extract
  6. extractionwas again extracted with water (30 mL)
  7. customThe combined water layer was evaporated to dryness
  8. customthe residue was crystallized with a mixture of acetonitrile and methyl tert-butyl ether