反应详情

温度

0 °C

To a suspension of LiAlH4 (0.83 g, 21.76 mmol) in tetrahydrofuran (50 ml) was added drop wise a solution of 2-ethyl-nicotinic acid ethyl ester (Breitmaier et al, Tetrahedron, 26, 1970, 5907-5910) (3 g, 16.74 mmol) in tetrahydrofuran (25 ml) at −50° C. After addition, the temperature was slowly allowed to increase to 0° C. After 3 h, the reaction was quenched with saturated NH4Cl, filtered and washed with 1M NaHCO3 (50 ml). The aqueous layer was extracted with ethyl acetate (3×50 ml). Combined organic extract were dried (Na2SO4), filtered and concentrated to yield 1.6 g (54%) of product as a yellowish liquid. MS (ESI+) m/z 138 (M+H)+;

1. additionAfter addition
2. customthe reaction was quenched with saturated NH4Cl
3. filtrationfiltered
4. washwashed with 1M NaHCO3 (50 ml)
5. extractionThe aqueous layer was extracted with ethyl acetate (3×50 ml)
6. extractionCombined organic extract
7. dry with materialwere dried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated