反应详情

N-(3,4Dimethoxybenzyl)-N-[thieno[2,3-d]pyrimidin-6-ylmethylidene]amine (intermediate 14) (76 mg), PhTosMIC (99 mg) and piperazine (31 mg) in THF (5 mL) were stirred under an inert atmosphere for 6 days. The reaction mixture was diluted with EtOAc and water. The organic layer was separated and the aqueous layer extracted with EtOAc (2×15 mL). The combined organics were dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluting with hexane:EtOAc (1:4) afforded the title compound as a pale yellow solid (50 mg, 48%);

1. customThe organic layer was separated
2. extractionthe aqueous layer extracted with EtOAc (2×15 mL)
3. dry with materialThe combined organics were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification by flash chromatography on silica eluting with hexane:EtOAc (1:4)