Water → 3-(Chloromethyl)-5-phenyl-1,2-oxazole
反応式
S(Cl)([Cl:3])=O.[C:5]1([C:11]2[O:15][N:14]=[C:13]([CH2:16]O)[CH:12]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.O>C1(C)C=CC=CC=1>[Cl:3][CH2:16][C:13]1[CH:12]=[C:11]([C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)[O:15][N:14]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
Thionyl chloride (7.55 ml) was added to a solution of (5-phenyl-3-isoxazolyl)methanol (12.1 g) in toluene (50 ml) and stirred at 80° C. for 3 hours. Water was added to the reaction mixture and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride, dried (MgSO4) and concentrated. The remaining crystals were recrystallized from ethyl acetate-hexane to obtain 3-(chloromethyl)-5-phenylisoxazole (11.8 g, yield 88%) as pale-yellow crystals. m.p. 46-47° C.
後処理
- extractionextracted with ethyl acetate
- washThe ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe remaining crystals were recrystallized from ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-8e496d887a9e480584154f7d4967fd30
- 出典データセット
- uspto-grants-2005_08
- 特許番号
- US06924300B2
反応ノート
読み込み中…