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

HRID 1820799노트

반응식

HRID 1820799 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-cd7628a6e40440948a66d5e1ce82a71e
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605163B2

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