Triethylamine → 4-(3-Chloro-propane-1-sulfonyl)-1,2-difluoro-benzene

HRID 1820799ノート

反応式

HRID 1820799 の反応式
[F:1][C:2]1[CH:3]=[C:4]([S:9]([OH:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].C(N(CC)CC)C.[Cl:19][CH2:20][CH2:21][CH2:22]I>CN(C=O)C>[Cl:19][CH2:20][CH2:21][CH2:22][S:9]([C:4]1[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=1)(=[O:11])=[O:10]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 813631-Chloro-3-iodopropaneHCID 138368283,4-Difluoro-benzenesulfinic acid

生成物 1

HCID 433451294-(3-Chloro-propane-1-sulfonyl)-1,2-difluoro-benzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 28.3 mmol 3,4-difluoro-benzenesulfinic acid and 36.8 mmol triethylamine in 100 ml DMF was added 70.7 mmol 1-chloro-3-iodopropane and the mixture stirred at RT for 1 h. The reaction mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were then washed with saturated aq. NaCl solution, dried over Na2SO4, and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane gradient) to afford the title compound.

後処理

  1. additionThe reaction mixture was then poured onto water
  2. extractionextracted three times with ethyl acetate
  3. washThe combined organic phases were then washed with saturated aq. NaCl solution
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed on silica gel (eluant: ethyl acetate/heptane gradient)

出典と根拠

ORDレコード
ord-cd7628a6e40440948a66d5e1ce82a71e
出典データセット
uspto-grants-2009_10
特許番号
US07605163B2

反応ノート

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