Phosphorus oxychloride → 4-Chloro-5-(4-methylphenyl)pyrimidine
反応式
O[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:6][N:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:6][N:5]=[CH:4][N:3]=1参加物
3
実験手順
A mixture of 4-hydroxy-5-(p-tolyl)pyrimidine (9 g, 48 mmol) and phosphorous oxychloride (44 ml) was heated under reflux for 2 hours. After the reaction mixture was concentrated to dryness, the residue was poured into iced water to precipitate crystals which were extraced with methylene chloride. The extract was washed with water, dried and concentrated to dryness. The residue was purified by column chromatography on silica gel to afford colorless powders (7 g, 71%), m.p. 67°-70° C.
後処理
- temperaturewas heated
- temperatureunder reflux for 2 hours
- concentrationAfter the reaction mixture was concentrated to dryness
- additionthe residue was poured into iced water
- customto precipitate crystals which
- washThe extract was washed with water
- customdried
- concentrationconcentrated to dryness
- customThe residue was purified by column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-676a0fad813844709279e9a036027c45
- 出典データセット
- uspto-grants-1995_02
- 特許番号
- US05389641
反応ノート
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