反应详情

温度

0 °C

A mixture of (3,4-dichlorophenyl)acetonitrile (0.149 mol) in DMF (100 ml) was stirred at 0° C. under N2 flow. Sodium hydride (0.223 mol) was added portionwise. The mixture was stirred at 0° C. under N2 flow for 1 hour. A mixture of, 2-methoxy-1,3-dimethyl-5-nitrobenzene (0.149 mol) in DMF (100 ml) was added dropwise at 0° C. under N2 flow. The mixture was stirred at RT for 6 hours, then cooled, hydrolized with H2O and with HCl 3N and extracted with EtOAc. The organic layer was separated, washed several times with H2O, dried, filtered and the solvent was evaporated. The residue was crystallized from DIPE. The precipitate was filtered off and dried, yielding 43.4 g (87%) of (±)-α-(3,4-dichlorophenyl)-2,6-dimethyl-4-nitrobenzeneacetonitrile (interm. 48).

1. stirringThe mixture was stirred at 0° C. under N2 flow for 1 hour
2. additionwas added dropwise at 0° C. under N2 flow
3. stirringThe mixture was stirred at RT for 6 hours
4. extractionextracted with EtOAc
5. customThe organic layer was separated
6. washwashed several times with H2O
7. customdried
8. filtrationfiltered
9. customthe solvent was evaporated
10. customThe residue was crystallized from DIPE
11. filtrationThe precipitate was filtered off
12. customdried