Thionyl Chloride → HCID 22221071, 화합물

HRID 1794323노트

반응식

HRID 1794323 반응식
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:13]([CH2:14]O)=[CH:12][O:11][N:10]=2)=[CH:5][CH:4]=1.S(Cl)([Cl:20])=O>>[Cl:20][CH2:14][C:13]1[C:9]([C:6]2[CH:7]=[CH:8][C:3]([C:2]([F:17])([F:16])[F:1])=[CH:4][CH:5]=2)=[N:10][O:11][CH:12]=1

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 22221163HCID 22221163, 화합물

생성물 1

HCID 22221071HCID 22221071, 화합물수율 95%

반응 조건

온도
0 °C

실험 절차

A mixture of 3-(4-trifluoromethylphenyl)-4-isoxazolylmethanol (6.00 g) and thionyl chloride (10.0 ml) was stirred at 0° C. for 30 min. The reaction mixture was concentrated, saturated aqueous sodium hydrogencarbonate was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained colorless crystals were filtrated to give 4-chloromethyl-3-(4-trifluoromethylphenyl)isoxazole (6.16 g, yield 95%). The crystals were recrystallized from ethyl acetate-hexane. melting point: 84–85° C.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionsaturated aqueous sodium hydrogencarbonate was added to the residue
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. filtrationThe obtained colorless crystals were filtrated

출처 및 근거

ORD 기록
ord-2a5c1d5d46c94e49885e5973f83659d4
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07022725B2

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