反应详情

To a stirred refluxing solution of sodium ethoxide (from 1.38 g sodium) in ethanol (25 ml) was added over 5 minutes a mixture of 2,3,5-trichlorophenylacetonitrile (11 g) and ethyl methoxyacetate (8.85 g) in dry DME (25 ml). After 4 hours the mixture was cooled on ice and acidified by dropwise addition of acetic acid (ca. 6 ml), diluted with ice-water (10 ml) and extracted with dichloromethane (2×100 ml). The dichloromethane extract was washed with water, dried over MgSO4 and concentrated giving a yellow solid, which was triturated with a little ether and filtered. 8.6 g Homogeneous by TLC (19:1 CH2Cl2 :MeOH).

1. additionwas added over 5 minutes
2. temperatureAfter 4 hours the mixture was cooled on ice
3. extractionextracted with dichloromethane (2×100 ml)
4. extractionThe dichloromethane extract
5. washwas washed with water
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customgiving a yellow solid, which
9. customwas triturated with a little ether
10. filtrationfiltered