HRID1374926
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewere heated
- temperatureIt was cooled to room temperature
- stirringwith stirring
- extractionThe solution was extracted with ether (30 mL)
- extractionThe ether extract
- extractionwas again extracted with water (30 mL)
- customThe combined water layer was evaporated to dryness
- customthe residue was crystallized with a mixture of acetonitrile and methyl tert-butyl ether