Thionyl Chloride → HCID 22221071、化合物

HRID 1794323ノート

反応式

HRID 1794323 の反応式
[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

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 22221163HCID 22221163、化合物

生成物 1

HCID 22221071HCID 22221071、化合物収率 95%

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2a5c1d5d46c94e49885e5973f83659d4
出典データセット
uspto-grants-2006_04
特許番号
US07022725B2

反応ノート

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