反应详情

To a cold suspension of anhydrous aluminum chloride (20 g, 75 mmol) in chlorobenzene 30 ml at 0° C. was added 1-methylpiperidine-4-carboxylic acid chloride in small portions and the resulted mixture was refluxed for 3 hours. The reaction mixture was cooled down, poured into ice water. The organic phase was discarded. The aqueous solution was washed with 2×50 ml ethyl ether, basified with potassium hydroxide pellet slowly to pH>10 and extracted with ethyl ether 4×50 ml. The combined organic solution was dried over sodium sulfate and concentrated to give 11.2 g of desired product in 85% yield.

1. temperaturethe resulted mixture was refluxed for 3 hours
2. temperatureThe reaction mixture was cooled down
3. washThe aqueous solution was washed with 2×50 ml ethyl ether
4. extractionextracted with ethyl ether 4×50 ml
5. dry with materialThe combined organic solution was dried over sodium sulfate
6. concentrationconcentrated