反应详情

A solution of 3-[2-[4-(2-methoxyphenyl)piperazin-1-yl]ethyl]thieno[3,2-d]pyrimidine-2,4-dione (2.6 g, 6.73 mmol) in acetic anhydride (30 ml) was heated to reflux for 5 hours. Acetic anhydride was removed in vacuo. The residue was dissolved in toluene, and the toluene was removed in vacuo. This process was repeated twice to remove any residual acetic anhydride. The residue was purified by flash chromatography on silica gel 60 (60 g) using 2.5% methanol in methylene chloride as eluant to give the product (1.65 g, 57% yield) as an off-white solid, mp 156°-158° C.

1. temperatureto reflux for 5 hours
2. customAcetic anhydride was removed in vacuo
3. dissolutionThe residue was dissolved in toluene
4. customthe toluene was removed in vacuo
5. customto remove any residual acetic anhydride
6. customThe residue was purified by flash chromatography on silica gel 60 (60 g)