反应详情

step 1—A 100 ml round bottom flask was charged under a stream of nitrogen with 3,5-dichlorobenzonitrile (R-3a,7.0 g, 40.69 mmol) and anhydrous DMF (75 mL). To the solution was added sodium methoxide (2.26 g, 44.76 mmol) and resulting solution was stirred further at RT for 24 h. When the reaction was complete, aqueous 10% HCl added dropwise to the reaction vessel. The crude mixture was extracted with EtOAc and sequentially washed with aqueous acid, water and brine. The EtOAc extracts were dried (Na2SO4), filtered and the solvent was removed in vacuo to afford a crude solid which was recrystallized from hexane/acetone to afford 5.9 g (86%) of 5-chloro-3-methoxy-benzonitrile.

1. customresulting solution
2. extractionThe crude mixture was extracted with EtOAc
3. washsequentially washed with aqueous acid, water and brine
4. dry with materialThe EtOAc extracts were dried (Na2SO4)
5. filtrationfiltered
6. customthe solvent was removed in vacuo
7. customto afford a crude solid which
8. customwas recrystallized from hexane/acetone