反应详情

Step B Add KCN (11.27 g, 0.173 mol) in water (25 mL) to a 100° C. solution of 4'-methoxychalcone (27.51 g 0.115 mol) and HOAc (7.5 mL, 0.128 mol) in 2-methoxyethanol (200 mL). The reaction is complete in <10 min. Cool the resulting solution to room temperature and pour into a mixture of ice and water (1 L). Extract the mixture with EtOAc. Combine the organic extracts, wash with water and brine, dry over Na2SO4, filter and concentrate in vacuo. Recrystallize the resulting solid from CH2Cl2 /MeOH to provide 23.07 g (75%) of 2-(4'-methoxyphenyl)-4-phenyl-3-oxobutyronitrile, mp 115°-116° C.

1. waitThe reaction is complete in <10 min
2. extractionExtract the mixture with EtOAc
3. washwash with water and brine
4. dry with materialdry over Na2SO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customRecrystallize the resulting solid from CH2Cl2 /MeOH