反应详情

A mixture of 2,4-diamino-5-[3,4-dimethoxy-5-(2-propynyloxy)benzyl]pyrimidine (1.18 g, 3.75 mmol), potassium carbonate (0.518 g, 3.75 mmol) and sulfolane (10 mL) was heated to 220°-230° under nitrogen over a period of 20 minutes and then maintained at this temperature for an additional 15 minutes. The resulting dark mixture was cooled and the precipitate was adsorbed on silica gel. The title compound was eluted with MeOH:CH2Cl2 /1:9 as an off-white powder, after recrystallization from 95% ethanol; mp 209°-212°. Anal. Calcd for C16H18N4O3.1/2H2O: C, 59.43; H, 5.92; N, 17.33. Found: C, 59.22; H, 5.97; N, 17.31.

1. temperaturewas heated to 220°-230° under nitrogen over a period of 20 minutes
2. temperaturemaintained at this temperature for an additional 15 minutes
3. temperatureThe resulting dark mixture was cooled
4. washThe title compound was eluted with MeOH
5. customCH2Cl2 /1:9 as an off-white powder, after recrystallization from 95% ethanol