反应详情

Add triethylamine (0.850 mL, 6.103 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 (10 mL). Stir at room temperature for 5 min. Add 4-fluoro-benzenesulfonyl chloride (0.356 g, 1.831 mmol) at room temperature. Stir at room temperature for 18 hr. Dilute with dichloromethane and saturated aqueous sodium bicarbonate. Separate the 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 (0.525 g, 83% yield). MS ES: m/z=413 [M+H]+.

1. customat room temperature
2. stirringStir at room temperature for 18 hr
3. customSeparate the phases
4. extractionextract the aqueous phase with dichloromethane
5. dry with materialdry over sodium sulfate
6. filtrationfilter
7. concentrationconcentrate
8. customPurify the resulting material by silica gel chromatography
9. washeluting with hexanes:acetone 1:1
10. customto afford the title
11. custompreparation (0.525 g, 83% yield)