反应详情

Suspend 4-cyanophenyl hydrazine hydrochloride (5 g, 29.58 mmol) in tert-butanol (60 mL). Add methoxyacrylonitrile (2.458 g, 29.58 mmol) and potassium tert-butoxide (3.975 g, 35.49 mmol) and heat the mixture at 90° C. overnight. Concentrate in vacuo and partition the residue between EtOAc/water. Extract the organic phase with 10% hydrochloric acid. Neutralize the aqueous phase with saturated aqueous NaHCO3 and extract twice with EtOAc. Dry the combined organic extracts over MgSO4, filter and concentrate in vacuo to obtain a solid that was washed with ether/hexane. Filter and dry the solid in vacuo to obtain the desired intermediate.

1. concentrationConcentrate in vacuo
2. custompartition the residue between EtOAc/water
3. extractionExtract the organic phase with 10% hydrochloric acid
4. extractionNeutralize the aqueous phase with saturated aqueous NaHCO3 and extract twice with EtOAc
5. dry with materialDry the combined organic extracts over MgSO4
6. filtrationfilter
7. concentrationconcentrate in vacuo
8. customto obtain a solid
9. washthat was washed with ether/hexane
10. filtrationFilter
11. customdry the solid in vacuo