反应详情

To a mixture of N-Hydroxy-2-phenyl-acetamidine (1 g, 6.7 mmol) in 7 mL ethyl acetate was added a solution of Chloro-oxo-acetic acid ethyl ester (1.5 g, 10.7 mmol) in 7 mL ethyl acetate at 0° C. The mixture was stirred for 1.5 h at room temperature and then heated to 80° C. for 2.5 h. The reaction mixture was treated with aq. NaHCO3-solution and extracted with ethyl acetate. The organic layers were dried over MgSO4 and evaporated in vacuo. The crude product was purified by preparative HPLC (Waters Sunfire Prep C18 PBD 5 um, 30×100 mm, 5 to 100% ACN and 0.1% TFA, flow 40ml/min) to yield the title compound. LCMS (method A) RtA=1.938 min; [M+H]+=233.1.

1. temperatureheated to 80° C. for 2.5 h
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layers were dried over MgSO4
4. customevaporated in vacuo
5. customThe crude product was purified by preparative HPLC (Waters Sunfire Prep C18 PBD 5 um, 30×100 mm, 5 to 100% ACN and 0.1% TFA, flow 40ml/min)