反应详情

3.81 ml of a cyclohexane solution of 1.75M of butyllithium were added at -30° to -40° C. to a mixture of 1.05 ml of diisopropylamine and 4 ml of tetrahydrofuran and the mixture was stirred for 10 minutes and was then cooled to -60° to -70° C. Then 1.22 g of p-tolyl isopropylsulfone were added to the mixture which after 15 minutes of contact was poured over 10 minutes under an inert atmosphere into a solution of 0.5 g of dimethylacrylonitrile and 4 ml of tetrahydrofuran at -60° to -70° C. The mixture was stirred for 30 minutes at -60° to -70° C. and was then poured into an aqueous saturated monosodium phosphate solution. The mixture was extracted with benzene and the organic phase was dried and evaporated to dryness. The residue was crystallized from isopropyl ether to obtain 0.740 g of 4-p-tolylsulfonyl-4,3,3,-trimethyl-pentanenitrile melting at 126° C.

1. temperaturewas then cooled to -60° to -70° C
2. stirringThe mixture was stirred for 30 minutes at -60° to -70° C.
3. extractionThe mixture was extracted with benzene
4. customthe organic phase was dried
5. customevaporated to dryness
6. customThe residue was crystallized from isopropyl ether