反应详情

温度

67.5 °C

A stirred mixture of 3-chloro-4-nitrobenzophenone (5.00 g), (J. Org. Chem., 1962, 27, 1605-1608), and copper(I)cyanide (2.57 g) in DMF (50 ml) was heated at reflux for 16 hours. The hot reaction mixture was then poured into a stirred solution of ferric chloride (15.30 g) concentrated hydrochloric acid (5 ml) and water (200 ml). The mixture was heated at 65-70° C. for 30 minutes, cooled to ambient temperature treated with ethyl acetate (250 ml) and stirred vigorously for 5 minutes. The organic phase was separated and the aqueous layer extracted with another 250 ml portion of ethyl acetate. The combined organics were dried, filtered and evaporated to give a brown oil. Chromatography (eluent toluene) gave the title compound (2.77 g) as a yellow solid. M.p. 117-119° C.; EA C14H8N2O3 requires C, 66.67; H, 3.02; N, 11.11%; found: C, 66.83; H, 2.99; N, 11.12%.

1. temperaturewas heated
2. temperatureat reflux for 16 hours
3. temperaturecooled to ambient temperature
4. customThe organic phase was separated
5. extractionthe aqueous layer extracted with another 250 ml portion of ethyl acetate
6. customThe combined organics were dried
7. filtrationfiltered
8. customevaporated
9. customto give a brown oil