反应详情

Methanamine (40% aq, 3 ml, 34.7 mmol) was added to a solution of 2-(2-{[5-(trifluoromethyl)pyridin-2-yl]methyl}cyclopentyl)-2,3-dihydro-1H-isoindole-1,3-dione (0.316 g, 0.84 mmol) in ethanol (5 ml). The reaction was stirred at room temperature for 24 hours and then further methanamine (40% aq, 3 ml, 34.7 mmol) was added. The reaction was stirred for 24 hours at room temperature and then re-suspended in ethanol (5 ml) and methanamine (40% aq, 3 ml, 34.7 mmol). The reaction stirred for 72 hours at room temperature. The reaction mixture was concentrated in vacuo and was then purified by reverse phase preparative HPLC (eluted with acetonitrile/water with 0.1% ammonia) and then purified by column chromatography (basic silica, 50-100% ethyl acetate/petrol) to afford the title compound.

1. stirringThe reaction was stirred for 24 hours at room temperature
2. stirringThe reaction stirred for 72 hours at room temperature
3. concentrationThe reaction mixture was concentrated in vacuo
4. customwas then purified by reverse phase preparative HPLC (eluted with acetonitrile/water with 0.1% ammonia)
5. custompurified by column chromatography (basic silica, 50-100% ethyl acetate/petrol)