反应详情

Couple 3′-(4-chlorophenyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.103 g, 0.400 mmol) and 3,5-dimethyl-1-phenyl 1H-pyrazole-4-carbaldehyde (0.083 g, 0.679 mmol) in the presence of acetic acid (0.035 mL, 0.61 mmol) and sodium triacetoxy-borohydride (0.105 g, 0.491 mmol) in DCE (5 mL) for 44 hr. Purify by silica gel chromatography, eluting with 0:100 to 10:90 methanol:DCM. Dissolve the free base in methanol and add ammonium chloride (6.0 mg, 0.2 mmol). Stir overnight, concentrate under reduced pressure, add diethyl ether and stir overnight. Isolate the solid product by filtration and vacuum dry overnight to give the title compound (0.0637 g, 46%). MS (ES): m/z=460 [M+H]+.

1. customPurify by silica gel chromatography
2. washeluting with 0:100 to 10:90 methanol
3. dissolutionDissolve the free base in methanol
4. concentrationconcentrate under reduced pressure
5. additionadd diethyl ether
6. stirringstir overnight
7. customIsolate the solid product
8. filtrationby filtration and vacuum
9. customdry overnight