反应详情

To a solution of 3′-chloro-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.789 g, 4.01 mmol) and 1-(2-hydroxy-ethyl)-1H-pyrazole-4-carbaldehyde (0.562 g, 4.01 mmol) in 1,2-dichloroethane (35 mL) add sodium triacetoxyborohydride (1.28 g, 6.02 mmol) and acetic acid (0.382 mL) and stir at room temperature for 20 hr. Add saturated aq. sodium bicarbonate, separate the layers, extract the aq. layer twice with DCM, dry (sodium sulfate), filter and concentrate. Purify using silica gel chromatography, eluting with 6:94 methanol (with 2 N ammonia): DCM to give 2-[4-(3′-chloro-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-ylmethyl)-pyrazol-1-yl]-ethanol as a yellow oil (1.16 g, 90%). MS (ES): m/z=323 [M+H]+.

1. customAdd saturated aq. sodium bicarbonate, separate the layers
2. extractionextract the aq. layer twice with DCM
3. dry with materialdry (sodium sulfate)
4. filtrationfilter
5. concentrationconcentrate
6. customPurify
7. washeluting with 6:94 methanol (with 2 N ammonia)