反应详情

Add triethylamine (0.426 mL, 3.058 mmol) to a stirring solution of [2-(3′-chloro-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-yl)-ethyl]-methyl-amine (0.200 g, 0.612 mmol) in dichloromethane (5 mL). Add pyridine-3-sulfonyl chloride hydrochloride salt (0.157 g, 0.734 mmol) at room temperature. Stir at room temperature for 20 min. Dilute with dichloromethane and saturated aqueous sodium bicarbonate. Separate and extract the aqueous fraction with dichloromethane. Combine the organic fractions, dry over sodium sulfate, filter, and concentrate. Purify the resulting material by silica gel chromatography eluting with hexanes:acetone 4:1 to afford the title preparation (0.220 g, 91% yield). MS ES: m/z=397 [M+H]+.

1. customat room temperature
2. customSeparate
3. extractionextract the aqueous fraction with dichloromethane
4. dry with materialdry over sodium sulfate
5. filtrationfilter
6. concentrationconcentrate
7. customPurify the resulting material by silica gel chromatography
8. washeluting with hexanes:acetone 4:1
9. customto afford the title
10. custompreparation (0.220 g, 91% yield)