Potassium Carbonate → 2-(4-Chlorobenzylthio)-ethyl 2-[4-(4-trifluoromethylphenoxy)-phenoxy]-propionate

HRID 65391노트

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HRID 65391 반응식
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:26]([CH3:41])[C:27]([O:29][CH2:30][CH2:31][S:32][CH2:33][C:34]1[CH:39]=[CH:38][C:37]([Cl:40])=[CH:36][CH:35]=1)=[O:28]>C(#N)C>[F:1][C:2]([F:17])([F:18])[C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:9]=[CH:10][C:11]([O:14][CH:26]([CH3:41])[C:27]([O:29][CH2:30][CH2:31][S:32][CH2:33][C:34]3[CH:35]=[CH:36][C:37]([Cl:40])=[CH:38][CH:39]=3)=[O:28])=[CH:12][CH:13]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 170230p-(4-(Trifluoromethyl)phenoxy)phenolHCID 133096322-{[(4-Chlorophenyl)methyl]sulfanyl}ethyl 2-bromopropanoate

생성물 1

HCID 133096052-(4-Chlorobenzylthio)-ethyl 2-[4-(4-trifluoromethylphenoxy)-phenoxy]-propionate수율 90.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture consisting of 25.4 g of 4-(4-trifluoromethylphenoxy)phenol, 14.5 g of anhydrous potassium carbonate, 33.8 g of 2-(4-chlorobenzylthio)ethyl 2-bromopropionate and 150 ml of dry acetonitrile was refluxed for 3 hours with vigorous stirring. After cooling the reaction mixture to room temperature, the acetonitrile was removed under reduced pressure. Then, 150 ml of toluene were added to the residue and the resulting mixture was washed successively with 1% strength by weight aqueous sodium hydroxide solution and water, followed by dehydration. Upon distilling off the toluene under reduced pressure, there were obtained 46.4 g of 2-(4-chlorobenzylthio)-ethyl 2-[4-(4-trifluoromethylphenoxy)-phenoxy]-propionate in the form of a colorless oil.

후처리

  1. temperaturewas refluxed for 3 hours with vigorous stirring
  2. customthe acetonitrile was removed under reduced pressure
  3. additionThen, 150 ml of toluene were added to the residue
  4. washthe resulting mixture was washed successively with 1% strength by weight aqueous sodium hydroxide solution and water
  5. distillationUpon distilling off the toluene under reduced pressure

출처 및 근거

ORD 기록
ord-de90401eb6a446af962bb59137c65cec
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614536

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