反应详情

A solution of ethyl 2-aminobenzoate (5.0 g, 30 mmol) in methoxyethanol (20 mL) was treated with formamidine acetate (8 g, 77 mmol) under reflux for 17 h. A second portion of formamidine acetate (8 g, 77 mmol) was then added, and the reflux was continued for 7 more hours. The mixture was cooled, and the solvent was removed under vacuum. The residue was taken in saturated NaHCO3 and extracted with ethyl acetate. The organic layers were combined, washed with saturated NaHCO3, and dried with magnesium sulfate, and the solvent was removed under vacuum to give the desired compound (4.84 g, 91%), which was used for the next step without further purification. LC-MS: m/z 147.7 (M+H)+

1. temperatureunder reflux for 17 h
2. temperatureThe mixture was cooled
3. customthe solvent was removed under vacuum
4. extractionextracted with ethyl acetate
5. washwashed with saturated NaHCO3
6. dry with materialdried with magnesium sulfate
7. customthe solvent was removed under vacuum