反应详情

温度

25 °C

To a stirred solution of 9.3 g (0.10 Mole) of aniline (IIIa) and 8.3 g (0.10 Mole) pyridine in 100 mL CH2Cl2 at 0° C. under an argon atmosphere was added a solution of 15.5 g (0.10 Mole) phenylacetyl chloride (IIa) in 25 mL CH2Cl2 over a 30 minute period. The solution was allowed to warm to 25° C. over 1 hour and was quenched into 200 mL H2O. The aqueous layer was washed with two 100 mL portions of CH2Cl2 and the combined organic layers were washed with two 100 mL portions of 10% HCl solution. The organic extract was dried over MgSO4, filtered, concentrated, and crystallized from CH2Cl2 /hexane to give 20.07 g (95%) of colorless needles. mp. 115°-116° C. δ1H-NMR (CDCl3) ppm 7.0-7.6 (m, 11 H); 3.67 (S, 2H).

1. customwas quenched into 200 mL H2O
2. washThe aqueous layer was washed with two 100 mL portions of CH2Cl2
3. washthe combined organic layers were washed with two 100 mL portions of 10% HCl solution
4. extractionThe organic extract
5. dry with materialwas dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customcrystallized from CH2Cl2 /hexane