Thionyl Chloride → 4-(Trifluoromethoxy)phenoxyacetyl chloride

HRID 1009193ノート

反応式

HRID 1009193 の反応式
[F:1][C:2]([F:16])([F:15])[O:3][C:4]1[CH:14]=[CH:13][C:7]([O:8][CH2:9][C:10](O)=[O:11])=[CH:6][CH:5]=1.S(Cl)([Cl:19])=O>CN(C=O)C>[F:1][C:2]([F:16])([F:15])[O:3][C:4]1[CH:14]=[CH:13][C:7]([O:8][CH2:9][C:10]([Cl:19])=[O:11])=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 6977052-(4-(Trifluoromethoxy)phenoxy)acetic acid

生成物 1

HCID 27773084-(Trifluoromethoxy)phenoxyacetyl chloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide触媒

実験手順

(4-Trifluoromethoxyphenoxy)-acetic acid (20.7 g, 88 mmol) was dissolved in thionyl chloride (100 mL). DMF (3 drops) was added to the solution. The solution was stirred for 14 hours. The thionyl chloride was removed in vacuo. The resulting oil was dissolved in dichloromethane, filtered through sodium sulfate and concentrate in vacuo to afford the title compound as a paste-like solid (21.8 g, 97% from the phenol): MS (EI-GCMS) for C9H6ClF3O3: 254 (M+).

後処理

  1. customThe thionyl chloride was removed in vacuo
  2. dissolutionThe resulting oil was dissolved in dichloromethane
  3. filtrationfiltered through sodium sulfate
  4. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-008a93ab7eb44053911af6dbbb4c8df6
出典データセット
uspto-grants-2011_07
特許番号
US07973061B2

反応ノート

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