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 DCE (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 aqueous sodium bicarbonate, separate the layers, extract the aqueous layer twice with DCM, dry (sodium sulfate), filter and concentrate. Purify using silica gel chromatography, eluting with 6:94 methanol (with 2N ammonia):DCM to give the title preparation as a yellow oil (1.16 g, 90%). MS (ES): m/z=323 [M+H]+.

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