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

HRID 1252647

반응식

HRID 1252647 반응식
[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

참가 물질

7

반응물 4

HCID 679Dimethyl SulfoxideHCID 94813,4-DichlorobenzotrifluorideHCID 11430Potassium CarbonateHCID 70420684HCID 70420684, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-fed63e1f15b146499654398b877f301e
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04744812

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