Phosphorus oxychloride → 2-Chloro-4-phenylthiazole
反応式
O[C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1参加物
3
実験手順
To 80 ml of phosphorus oxychloride were added 7.7 g (43 mmol) of 2-hydroxy-4-phenylthiazole, followed by heating at 100°-105° C. for 2 hours. The solvent was then distilled off from the reaction mixture under reduced pressure. Ice water was added to the residue, followed by extraction with ethyl ether. The ether layer was washed with water. After purification by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1), the title compound was obtained as pale yellow crystals.
後処理
- temperatureby heating at 100°-105° C. for 2 hours
- distillationThe solvent was then distilled off from the reaction mixture under reduced pressure
- additionIce water was added to the residue
- extractionfollowed by extraction with ethyl ether
- washThe ether layer was washed with water
- customAfter purification by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1)
出典と根拠
- ORDレコード
- ord-bbd48428ddad4311a4e64414339d0545
- 出典データセット
- uspto-grants-1992_05
- 特許番号
- US05112841
反応ノート
読み込み中…