Water → 3-(Chloromethyl)-5-phenyl-1,2-oxazole
반응식
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]=1참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-8e496d887a9e480584154f7d4967fd30
- 출처 데이터셋
- uspto-grants-2005_08
- 특허 번호
- US06924300B2
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