反应详情

Under argon gas, 4,4-diphenyl-4-formylbutanenitrile (5.0 g) was dissolved in dry tetrahydrofuran (200 ml). Then, 1M vinylmagnesium bromide-tetrahydrofuran (30 ml) was added dropwise -40° C. After completion of addition, the reaction temperature was allowed to rise gradually to 0° C. (over 3 hours). After completion of the reaction, a saturated aqueous solution of ammonium chloride was added to the reaction mixture and the insoluble matter was filtered off. The filtrate was extracted with ethyl acetate, washed, dried, and concentrated and the group was purified by silica gel column chromatography. The active fraction was concentrated to provide the title compound as oil (5.4 g).

1. additionAfter completion of addition
2. customto rise gradually to 0° C.
3. custom(over 3 hours)
4. customAfter completion of the reaction
5. filtrationthe insoluble matter was filtered off
6. extractionThe filtrate was extracted with ethyl acetate
7. washwashed
8. customdried
9. concentrationconcentrated
10. customthe group was purified by silica gel column chromatography
11. concentrationThe active fraction was concentrated