反应详情

To a mixture of 7.73 g of 2-chloro-N-(3,4-dimetoxyphenethyl)acetamide, 5.12 g of 2-amino-4-chlorobenzamide, 13.5 g of sodium iodide and 3.63 g of magnesium oxide was added 30 ml of dimethylformamide and the resulting mixture was stirred at 90° to 100° C. for 4.5 hours. The reaction solution was concentrated under reduced pressure and the residue was extracted with 500 ml of chloroform. The chloroform extract was washed successively with 10% hydrochloric acid, water, a 5% aqueous sodium carbonate solution, a 5% aqueous sodium sulfite solution and water, dried and then concentrated to dryness under reduced pressure. The residue was recrystallized from methanol to obtain 8.01 g of 2-(2-carbamoyl-5-chlorophenylamino)-N-(3,4-dimethoxyphenethyl)acetamide having a melting point of 167.5°-168.5° C.

1. concentrationThe reaction solution was concentrated under reduced pressure
2. extractionthe residue was extracted with 500 ml of chloroform
3. extractionThe chloroform extract
4. washwas washed successively with 10% hydrochloric acid, water
5. dry with materiala 5% aqueous sodium carbonate solution, a 5% aqueous sodium sulfite solution and water, dried
6. concentrationconcentrated to dryness under reduced pressure
7. customThe residue was recrystallized from methanol