反应详情

A mixture of 11 g of Raney nickel, 8.2 g of 4'-cyano-2',3'-difluoroacetanilide and 125 mL of 95% HCOOH is stirred and heated 30 minutes at 80°-85° C. The hot solution is filtered through diatomaceous earth and the cake washed with 3×100 mL of CH2CL2. The filtrate and wash are evaporated in vacuo to furnish a white solid. Excess saturated NaHCO3 is added to neutralize the residual HCOOH and the product is extracted with 3×400 mL of CH2Cl2. The CH2Cl2 extract is washed with saturated NaHCO3 and H2O (100 mL each), dried with Na2SO4 and evaporated to furnish 7.7 g (92.5% yield) of 2',3'-difluoro-4'-formylacetanilide, m.p. 154° C. The mass spectrum shows an ion at 200.

1. temperatureheated 30 minutes at 80°-85° C
2. filtrationThe hot solution is filtered through diatomaceous earth
3. washthe cake washed with 3×100 mL of CH2CL2
4. washThe filtrate and wash
5. customare evaporated in vacuo
6. customto furnish a white solid
7. extractionthe product is extracted with 3×400 mL of CH2Cl2
8. extractionThe CH2Cl2 extract
9. washis washed with saturated NaHCO3 and H2O (100 mL each)
10. dry with materialdried with Na2SO4
11. customevaporated