反应详情

To a stirred solution of 3-(pyrazin-2-yl)benzaldehyde [376637-85-3] (200 mg, 1.09 mmol) in methanol (5 mL), NaBH4 (82 mg, 2.17 mmol) was added at 0° C. and stirred for 10 min. Then the mixture was allowed to warm to rt and stirred for 3 h. The mixture was concentrated under reduced pressure at 45° C., saturated aqueous NH4Cl solution was added and extracted with ethyl acetate (2×5 mL). The combined organic layers were washed with brine and dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to yield the title compound as a liquid (200 mg, 99%). [LCMS RtE=0.20 min, [M+H]+=187.0; TLC Rf=0.26 (ethyl acetate/hexane 50:50)].

1. stirringstirred for 3 h
2. concentrationThe mixture was concentrated under reduced pressure at 45° C.
3. additionsaturated aqueous NH4Cl solution was added
4. extractionextracted with ethyl acetate (2×5 mL)
5. washThe combined organic layers were washed with brine
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure