反应详情

7-Bromothieno[3,2-d]pyrimidin-4(3H)-one (0.9 g, 3.89 mmol) in POCl3 was heated under reflux for 2 hours and excess of POCl3 was removed under reduced pressure. The residue was partitioned between water and EtOAc. The organic layer was separated, and the aqueous layer was extracted with additional EtOAc. The combined organic layers were washed with brine, dried (MgSO4), filtered, and concentrated to give 0.91 g of the compound 65A: 1H NMR (DMSO-d6): δ 9.15 (s, 1H), 8.78 (s, 1H). ESI (+)/MS: 248 (M−H)+.

1. customwas removed under reduced pressure
2. customThe residue was partitioned between water and EtOAc
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with additional EtOAc
5. washThe combined organic layers were washed with brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated