反应详情

Add triethylamine (3.403 mL, 24.414 mmol) to a stirring solution of {2-[4-(2-chloro-pyridin-3-yl)-piperazin-1-yl]-ethyl}-methyl-amine hydrochloride salt (2.000 g, 6.103 mmol) in dichloromethane (100 mL). Add 1-methyl-1H-pyrazole-4-sulfonyl chloride (1.102 g, 6.103 mmol) at room temperature. Stir at room temperature for 30 min. Dilute with dichloromethane and saturated aqueous sodium bicarbonate. Separate phases and extract the aqueous phase with dichloromethane. Combine the organic phases, dry over sodium sulfate, filter, and concentrate. Purify the resulting material by silica gel chromatography eluting with hexanes:acetone 1:1 to afford the title preparation (1.600 g, 66% yield). MS ES: m/z=399 [M+H]+.

1. customat room temperature
2. extractionSeparate phases and extract the aqueous phase with dichloromethane
3. dry with materialdry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate
6. customPurify the resulting material by silica gel chromatography
7. washeluting with hexanes:acetone 1:1
8. customto afford the title
9. custompreparation (1.600 g, 66% yield)