反应详情

温度

50 °C

100 mg (0.427 mmol) of 2,N-dimethyl-5-morpholin-4-ylbenzamide prepared in Step A was dissolved in 3 ml of N,N-dimethylformamide, and thereafter, 63 mg (0.47 mmol) of N-chlorosuccinimide was added thereto under cooling on ice. The obtained mixture was stirred at 50° C. for 1 hour. Thereafter, the reaction solution was concentrated, and water was then added thereto. The mixture was extracted with ethyl acetate. The extract was washed with water and a saturated saline solution, and was then dried over anhydrous sodium sulfate. The extract was concentrated, and the obtained residue was then purified by silica gel column chromatography (ethyl acetate:methylene chloride=1:5), so as to obtain 54.5 mg (47%) of 4-chloro-2,N-dimethyl-5-morpholin-4-ylbenzamide in the form of a colorless solid, as well as 46 mg (40%) of 2-chloro-6,N-dimethyl-3-morpholin-4-ylbenzamide in the form of a colorless solid.

1. temperatureunder cooling on ice
2. concentrationThereafter, the reaction solution was concentrated
3. additionwater was then added
4. extractionThe mixture was extracted with ethyl acetate
5. washThe extract was washed with water
6. dry with materiala saturated saline solution, and was then dried over anhydrous sodium sulfate
7. concentrationThe extract was concentrated
8. customthe obtained residue was then purified by silica gel column chromatography (ethyl acetate:methylene chloride=1:5)