反应详情

Add triethylamine (0.852 mL, 6.116 mmol) to a stirring solution of [2-(3′-chloro-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-yl)-ethyl]-methyl-amine (0.500 g, 1.529 mmol) in dichloromethane (10 mL). Add 1-methyl-1H-pyrazole-4-sulfonyl chloride (0.331 g, 1.834 mmol) at room temperature. Stir at room temperature for 18 hr. Dilute with dichloromethane and saturated aqueous sodium bicarbonate. Separate and extract the aqueous layer with dichloromethane. Combine the organic layers, dry over sodium sulfate, filter, and concentrate. Purify the resulting material by silica gel chromatography eluting with hexanes:acetone 6:4 to 4:6 to afford the title preparation (0.514 g, 84% yield). MS ES: m/z=400 [M+H]+.

1. customat room temperature
2. customSeparate
3. extractionextract the aqueous layer 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 6:4 to 4:6
9. customto afford the title
10. custompreparation (0.514 g, 84% yield)