Hydrochloric Acid → 4-Fluoro-2-benzoylthiophenol

HRID 1716197노트

반응식

HRID 1716197 반응식
F[C:2]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[S-2:17].[Li+].[Li+].Cl.C(OCC)(=O)C>CS(C)=O.O>[F:16][C:13]1[CH:14]=[CH:15][C:2]([SH:17])=[C:3]([C:4](=[O:5])[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH:12]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 5228262,5-DifluorobenzophenoneHCID 10290727Dilithium Sulfide

생성물 1

HCID 230742324-Fluoro-2-benzoylthiophenol수율 98%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

To a solution of 10.1 g of 2,5-difluorobenzophenone in 200 ml of DMSO was added 3.5 g of lithium sulfide (manufactured by ALDRICH CHEMICAL COMPANY) and the mixture was stirred in a nitrogen atmosphere at 120° C. for 3 hours. To the reaction solution was added 200 ml of 1N hydrochloric acid under ice cooling, and further 400 ml of ethyl acetate and 200 ml of water were added to the mixture to separate it. The organic layer was washed with 400 ml of water and then with 200 ml of saturated saline. The organic layer was dried over anhydrous sodium sulfate and then concentrated to obtain 10.54 g of the title compound.

후처리

  1. customto separate it
  2. washThe organic layer was washed with 400 ml of water
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-15fed540865d4c7ea9b9da66f2fe5595
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803792B2

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