反应详情

To a solution of 4-(4-chlorophenyl)-1,2-butanediamine (0.084 mg, 0.42 mmol) in ethanol (8 ml) was added formamidine acetate (0.15 g, 1.45 mmol) and the mixture was stirred overnight at room temperature. The solvent was evaporated, water (5 ml) was added and the mixture was extracted 3 times with dichloromethane (10 ml). The combined organic layers were dried over magnesium sulfate and evaporated. The residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10) to yield an off-white amorphous solid (0.041 g, 47%); MS (ISP): 209.3 ((M+H)+).

1. customThe solvent was evaporated
2. additionwater (5 ml) was added
3. extractionthe mixture was extracted 3 times with dichloromethane (10 ml)
4. dry with materialThe combined organic layers were dried over magnesium sulfate
5. customevaporated
6. customThe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10)