Hydrochloric Acid → 4-Fluoro-2-benzoylthiophenol

HRID 1008754노트

반응식

HRID 1008754 반응식
[S-2:1].[Li+].[Li+].F[C:5]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:6]=1[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8].Cl.C(OCC)(=O)C>CS(C)=O.O>[F:19][C:16]1[CH:17]=[CH:18][C:5]([SH:1])=[C:6]([C:7](=[O:8])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:15]=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

Lithium sulfide (3.5 g) (supplied from Aldrich) was added to a solution of 10.1 g of 2,5-difluorobenzophenone in 200 mL of DMSO, and stirred at 120° C. under a nitrogen atmosphere for 3 hours. Under ice cooling, 200 mL of 1 N hydrochloric acid was added to the reaction solution. Further 400 mL of ethyl acetate and 200 mL of water were added thereto, and the mixture was separated into two liquid phases. The organic layer was washed with 400 mL of water, and then washed with 200 mL of saturated brine. The organic layer was dried on sodium sulfate anhydrate and subsequently concentrated, to yield 10.54 g of the title compound.

후처리

  1. customthe mixture was separated into two liquid phases
  2. washThe organic layer was washed with 400 mL of water
  3. washwashed with 200 mL of saturated brine
  4. customThe organic layer was dried on sodium sulfate anhydrate
  5. concentrationsubsequently concentrated

출처 및 근거

ORD 기록
ord-ab1e9b158bf64d56b9b3cccafe0deb55
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973030B2

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