Dimethyl Sulfoxide → Benzene, 2-Chloro-1-(3-methylphenoxy)-4-(trifluoromethyl)-

HRID 1252647

反応式

HRID 1252647 の反応式
[C:1]1(C([O-])=O)[C:2]([CH3:8])=[CH:3][CH:4]=[CH:5][C:6]=1[OH:7].[K+].[Cl:13][C:14]1[CH:15]=[C:16]([C:21]([F:24])([F:23])[F:22])[CH:17]=[CH:18][C:19]=1Cl.C(=O)([O-])[O-].[K+].[K+].CS(C)=O>CCOCC.O>[Cl:13][C:14]1[CH:15]=[C:16]([C:21]([F:22])([F:23])[F:24])[CH:17]=[CH:18][C:19]=1[O:7][C:6]1[CH:1]=[C:2]([CH3:8])[CH:3]=[CH:4][CH:5]=1

参加物

7

反応物 4

HCID 679Dimethyl SulfoxideHCID 94813,4-DichlorobenzotrifluorideHCID 11430Potassium CarbonateHCID 70420684HCID 70420684、化合物

生成物 1

HCID 3084880Benzene, 2-Chloro-1-(3-methylphenoxy)-4-(trifluoromethyl)-収率 84%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

73 parts by weight of potassium 3-cresolate, 107 parts by weight of 3,4-dichlorobenzotrifluoride and 6.9 parts by weight of potassium carbonate in 500 parts by volume of dimethylsulfoxide were stirred at 140° C. for 8 hours. The reaction mixture was cooled to room temperature and was poured into 2,000 parts by volume of water. The oily residue was taken up in ether, and the organic phase was dried with magnesium sulfate, filtered, and concentrated under reduced pressure. Fractional distillation gave 120 parts by weight (84% of theory) of 3-(2'-chloro-4'-trifluoromethylphenoxy)-toluene of boiling point 91°-96° C./0.1 bar and refractive index nD25 : 1.5268.

後処理

  1. dry with materialthe organic phase was dried with magnesium sulfate
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. distillationFractional distillation

出典と根拠

ORDレコード
ord-fed63e1f15b146499654398b877f301e
出典データセット
uspto-grants-1988_05
特許番号
US04744812

関連ノート

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