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
- 0 °C
PROCEDURE
实验过程
A mixture of aluminum chloride(III) (26 g, 195 mmol) and dichloromethane (200 mL) was stirred at 0° C., and oxalyl chloride (20 mL, 228 mmol) was dripped over 10 minutes. Then a mixture of 1-(4-phenylpiperidin-1-yl)ethanone described in Production Example 1-9 (12.3 g, 60.5 mmol) and dichloromethane (50 mL) was dripped over 30 minutes. The mixture was stirred under nitrogen atmosphere at 25° C. for 14 hours. The reaction liquid was poured onto ice and ethyl acetate (1 L) and water (1 L) were added for separation. The aqueous layer was extracted with ethyl acetate (1 L) twice, then the organic layer was washed with water (1 L) twice and then with a saturated saline solution (500 mL). The organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated. Ethyl acetate was added to the concentrated residue and the product was collected by filteration and washed with ethyl acetate to obtain the title compound (9.09 g, 61%).
WORKUP
后处理
- stirringThe mixture was stirred under nitrogen atmosphere at 25° C. for 14 hours
- customThe reaction liquid
- additionwere added for separation
- extractionThe aqueous layer was extracted with ethyl acetate (1 L) twice
- washthe organic layer was washed with water (1 L) twice
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- customthe solvent was evaporated
- additionEthyl acetate was added to the concentrated residue
- customthe product was collected by filteration
- washwashed with ethyl acetate