Phosphorus oxychloride → 2-Chloro-4-phenylthiazole
反応式
[C:1]1([C:7]2[N:8]=[C:9](O)[S:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:9]1[S:10][CH:11]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:8]=1参加物
3
実験手順
A mixed solution of 4-phenyl-1,3-thiazol-2-ol (2.00 g, 11.3 mmol) in phosphorus oxychloride (20 ml) was stirred at 100° C. for 2 hours. The solvent was distilled off under reduced pressure. The residue was poured to ice water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to give 1.44 g (65.2%) of the desired product as a solid.
後処理
- distillationThe solvent was distilled off under reduced pressure
- additionThe residue was poured to ice water
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)
出典と根拠
- ORDレコード
- ord-41fa803d4b4941b2aba444587b98589a
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07851473B2
反応ノート
読み込み中…