Ethanethiol → 2-(Ethylthio)-4-(trifluoromethyl)benzoic acid

HRID 1052926노트

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HRID 1052926 반응식
[CH2:1]([SH:3])[CH3:2].F[C:5]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8].C(=O)([O-])[O-].[Cs+].[Cs+].C(=O)(O)[O-].[Na+]>CN1C(=O)CCC1>[CH2:1]([S:3][C:5]1[CH:13]=[C:12]([C:14]([F:15])([F:17])[F:16])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])[CH3:2]

참가 물질

6

반응물 4

HCID 6343EthanethiolHCID 10796Cesium carbonateHCID 516892Sodium BicarbonateHCID 5180032-Fluoro-4-(trifluoromethyl)benzoic acid

생성물 1

HCID 918763722-(Ethylthio)-4-(trifluoromethyl)benzoic acid

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
60 °C

실험 절차

1.5 mL of ethyl mercaptan was added to a mixture of 3.83 g of 2-fluoro-4-trifluoromethylbenzoic acid, 10 mL of NMP and 15 g of cesium carbonate, and the mixture was stirred at 60° C. for 4 hours. A saturated aqueous sodium bicarbonate solution was added to the cooled reaction mixture, and the mixture was extracted with ethyl acetate. Hydrochloric acid was added to the aqueous layer, and the precipitated solid was taken by filtration and dried under reduced pressure to obtain 4.6 g of 2-ethylsulfanyl-4-trifluoromethylbenzoic acid.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. additionHydrochloric acid was added to the aqueous layer
  3. filtrationthe precipitated solid was taken by filtration
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-05a4ebb12e1748c8b60144b170c19cf8
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09392791B2

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