반응 #72425
ord-d035fcd97bf94e418daadc8bb68dc8cf
반응 조건
온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과filtered
- 2기타to remove selenium waste
- 3농축The filtrate was concentrated
- 4기타to give a residue that
- 5여과the precipitated solid was filtered
- 6세척washed with acetone (2×20 mL)
- 7기타dried
- 8기타to provide (BB12) (3.1 g, 58%) as a brown solid
실험 절차
To a solution of 4-methylpyrimidine (4 g, 46.5 mmol) in pyridine (20 mL) was added SeO2 (8.7 g, 79.06 mmol) at room temperature. The reaction mixture was then heated to 60° C. for 2 h, and then stirred at room temperature for 16 h. The reaction mixture was diluted with DCM (50 mL) and filtered to remove selenium waste. The filtrate was concentrated to give a residue that was stirred with H2O (20 mL), the precipitated solid was filtered and washed with acetone (2×20 mL) and dried to provide (BB12) (3.1 g, 58%) as a brown solid. Rf: 0.2 (40% MeOH/CHCl3). 1H NMR (400 MHz, DMSO-d6): δ 13.8 (1H, br s), 9.37 (1H, s), 9.07 (1H, d, J=5.2 Hz), 8.01 (1H, d, J=4 Hz); m/z 123 (M−H)−.