Hydrochloric Acid → 4-Fluoro-2-benzoylthiophenol

HRID 1008751

反応式

HRID 1008751 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 230742324-Fluoro-2-benzoylthiophenol収率 98%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e6862eb614de44248cafca7a25714573
出典データセット
uspto-grants-2011_07
特許番号
US07973030B2

関連ノート

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