反应详情

Dissolve (2-{4-[3′-(4-fluoro-phenyl)-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-ylmethyl]-pyrazol-1-yl}-ethyl)-methyl-amine (0.124 g, 0.314 mmol) in DCM (3 mL) with triethylamine (66 μL, 0.470 mmol). Add methanesulfonyl chloride (26 μL, 0.329 mmol) dropwise in DCM (1 mL). Stir the mixture for 20 hr. Dilute with saturated aqueous sodium bicarbonate then extract 3 times with DCM. Dry (sodium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 4.5:95.5 2 M ammonia in methanol:DCM), to give a yellow oil. Dissolve the oil in methanol and add ammonium chloride then sonicate the mixture for 10 min. Evaporate the solution to give the title compound as a yellow solid (0.154 g, 97%). MS (ES): m/z=474 [M+H]+.

1. extractionthen extract 3 times with DCM
2. dry with materialDry (sodium sulfate)
3. filtrationfilter
4. concentrationconcentrate
5. custompurify
6. wash(silica gel chromatography, eluting with 4.5:95.5 2 M ammonia in methanol:DCM)
7. customto give a yellow oil
8. customthen sonicate the mixture for 10 min
9. customEvaporate the solution