Phosphorus oxychloride → 4-Chloro-2-methyl-6-phenylpyrimidine
反応式
[CH3:1][C:2]1[NH:7][C:6](=O)[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:6]1[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=[C:2]([CH3:1])[N:7]=1参加物
3
実験手順
A mixture of 2-methyl-6-phenylpyrimidin-4(3H)-one (15 g) and POCl3 (150 ml) was refluxed under nitrogen for 20 h. The excess POCl3 was distilled off and the residue was diluted with ethyl acetate (500 ml) and washed with 10% solution of sodium bicarbonate (100 ml), water, brine and dried. The solvent was removed under reduced pressure and the residue was purified by chromatography (silica, 60-120 mesh) eluting with pet ether/ethyl acetate (9/1) to afford 11 g (67%) of the titled as a pale yellow solid.
後処理
- temperaturewas refluxed under nitrogen for 20 h
- distillationThe excess POCl3 was distilled off
- additionthe residue was diluted with ethyl acetate (500 ml)
- washwashed with 10% solution of sodium bicarbonate (100 ml), water, brine
- customdried
- customThe solvent was removed under reduced pressure
- customthe residue was purified by chromatography (silica, 60-120 mesh)
- washeluting with pet ether/ethyl acetate (9/1)
- customto afford 11 g (67%) of the
出典と根拠
- ORDレコード
- ord-3eb7dbdd86134f718aec396d3c97aa72
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08288398B2
反応ノート
読み込み中…