反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
To a stirred suspension of K2CO3 (4.5 g, 32.6 mmol) and cyclohexylmercaptan (2.0 mL, 16.4 mmol) in DMSO (20 mL) was added 2-fluorobenzaldehyde (1.7 mL, 16.2 mmol) dropwise over 10 minutes at room temperature, and the reaction mixture was heated at 100° C. for 5 hours with stirring. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and water. The organic layer was separated and the aqueous phase extracted with ethyl acetate (×3). The combined organic extracts were washed successively with sodium bicarbonate solution and brine, then dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo to afford 2-(cyclohexylthio)benzaldehyde (3.22 g, 14.6 mmol, 90%) which was used directly without further purification.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customthe reaction mixture was partitioned between ethyl acetate and water
- customThe organic layer was separated
- extractionthe aqueous phase extracted with ethyl acetate (×3)
- washThe combined organic extracts were washed successively with sodium bicarbonate solution and brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo