HRID1881683
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 4-(2-piperidinyl)butanoic acid hydrochloride (5.95 g, 34.8 mmol) in methanol (104 ml) was cooled to 0° C. Thionyl chloride (7.54 ml, 104.3 mmol) was slowly added at this temperature. The reaction mixture was heated under reflux for 12 h. The solvent was evaporated off under reduced pressure. The residue was suspended in ethyl acetate and the suspension was heated under reflux. The suspension was filtered hot. A white precipitate precipitates out in the filtrate, and was filtered out and dried under reduced pressure to give the product methyl 4-(piperidine-2-yl)butanoate hydrochloride (2) (3.49 g, 45%).
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 12 h
- customThe solvent was evaporated off under reduced pressure
- temperaturethe suspension was heated
- temperatureunder reflux
- filtrationThe suspension was filtered hot
- customA white precipitate precipitates out in the filtrate
- filtrationwas filtered out
- customdried under reduced pressure