反应详情

N-(4-Methoxy-7-morpholin-4-yl-benzothiazol-2-yl)-2-methylaminomethyl-isonicotinamide (207 mg, 0.5 mmol) is dissolved in dichloromethane (10 ml) and treated with pyridine (0.07 ml, 0.85 mmol) and acetyl chloride (0.05 ml, 0.7 mmol) and stirred for 16 h at ambient temperature. Saturated aqueous sodium hydrogen carbonate (10 ml) is added, the layers are separated and the aqueous phase extracted twice with each 10 ml dichloromethane. The combined organic phases are dried with magnesium sulfate and evaporated. Recrystallization from ethyl acetate afforded the title compound as light-yellow solid (80% yield), mp 228-230° C. MS: m/e=456 (M+H+).

1. customthe layers are separated
2. extractionthe aqueous phase extracted twice with each 10 ml dichloromethane
3. dry with materialThe combined organic phases are dried with magnesium sulfate
4. customevaporated
5. customRecrystallization from ethyl acetate