반응 #1546
ord-d6194f9ae43e4fbd94964245b6b3d3e4
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was heated to reflux
- 2온도The mixture was maintained
- 3온도at reflux for 2 h
- 4온도cooled
- 5여과filtered
- 6기타to remove unreacted zinc
- 7기타to leave a semi-solid which
- 8기타was triturated with 75 mL of boiling water
실험 절차
A mixture of 7.07 g (18.1 mmol) of crude 5-iodo-6-phenoxy-2-phenyl-4(3H)-pyrimidinone, 2.02 g (31.1 mmol) of zinc dust and 25 mL of glacial acetic acid was heated to reflux. After 15 min an additional 2.06 g (31.7 mmol) of zinc dust was added, followed 15 min later by a further 2.04 g (31.4 mmol) of zinc dust. The mixture was maintained at reflux for 2 h, cooled and filtered to remove unreacted zinc. The filtrate was rotovaped to leave a semi-solid which was triturated with 75 mL of boiling water to afford 6.01 g (57% from 4,6-dihydroxy-2-phenylpyrimidine) of 6-phenoxy-2-phenyl-4(3H)-pyrimidinone as a yellow solid. 1H-NMR (d6-DMSO) δ 5.5(1H,s), 7.1-7.5(8H), 8.1(2H).