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Dimethylformamide → 2-[4-(4-Chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride

HRID 973301
ノート
印刷プレビュー

反応式

HRID 973301 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:27]=[CH:26][C:11]([CH2:12][O:13][C:14]([C:22]([F:25])([F:24])[F:23])([C:18]([F:21])([F:20])[F:19])[C:15](O)=[O:16])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.S(Cl)([Cl:30])=O.CN(C)C=O>C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]([CH2:12][O:13][C:14]([C:18]([F:19])([F:20])[F:21])([C:22]([F:24])([F:25])[F:23])[C:15]([Cl:30])=[O:16])=[CH:26][CH:27]=2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 133842612-[4-(4-Chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionic acid

生成物 1

HCID 203144652-[4-(4-Chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionic acid (3.0 g.), thionyl chloride (3.0 ml.), dimethylformamide (0.16 g.) and benzene (10 ml.) is heated under reflux until the solution becomes turbid (ca. 10 minutes). The mixture is evaporated in vacuo, benzene (10 ml.) is added and the evaporation is repeated. Light petroleum (10 ml., b.p. 40°-60° C.) is added to the residue, and the solution is separated from insoluble oils and evaporated to give 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride (3.07 g.), m.p. 30°-35° C.

後処理

  1. temperatureis heated
  2. temperatureunder reflux until the solution
  3. customturbid (ca. 10 minutes)
  4. customThe mixture is evaporated in vacuo, benzene (10 ml.)
  5. additionis added
  6. customthe evaporation
  7. additionLight petroleum (10 ml., b.p. 40°-60° C.) is added to the residue
  8. customthe solution is separated from insoluble oils
  9. customevaporated

出典と根拠

ORDレコード
ord-06d23d95d060492fb7ff67b56559362d
出典データセット
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04055595

反応ノート

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