反应详情

250 mg 4-methyl-1-pyrimidin-2-yl-1H-pyrrole-3-carboxylic acid methyl ester was dissolved in 0.3 mL of NMP. After addition of 1 g guanidine (preparation according to known literature) the mixture was heated under argon for 1 h to 90° C. Completion of the reaction was checked by LCMS. The mixture was cooled to room temperature and then diluted with water, followed by extraction with ethyl acetate. The organic layer was washed with water (twice), dried over anhydrous sodium sulfate. After filtration the solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column flash chromatography (eluent: dichloromethane/methanol=5/1) to obtain 150 mg of N-(4-methyl-1-pyrimidin-2-yl-1H-pyrrole-3-carbonyl)-guanidine.

1. temperaturewas heated under argon for 1 h to 90° C
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with water (twice),
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfter filtration the solvent
6. distillationwas distilled off under reduced pressure
7. customthe resulting residue was purified by a silica gel column flash chromatography (eluent: dichloromethane/methanol=5/1)