Methyl iodide → 6-(4-(2-(N-Methyl-4-chlorobenzenesulphonylamino)ethyl)phenyl)-6-(3-pyridyl)hex-5-enoic acid

HRID 1490381

반응식

HRID 1490381 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)=[CH:21][CH2:22][CH2:23][CH2:24][C:25]([OH:27])=[O:26])=[CH:16][CH:15]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH2:34](Cl)Cl.CI>[OH-].[Na+].[Cl-].C([N+](C)(C)C)C1C=CC=CC=1>[CH3:34][N:11]([S:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)(=[O:9])=[O:10])[CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([C:28]2[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=2)=[CH:21][CH2:22][CH2:23][CH2:24][C:25]([OH:27])=[O:26])=[CH:16][CH:15]=1

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 6344DichloromethaneHCID 659716-(4-(2-(4-Chlorobenzenesulphonylamino)ethyl)-phenyl)-6-(3-pyridyl)hex-5-enoic acid

생성물 1

HCID 542628046-(4-(2-(N-Methyl-4-chlorobenzenesulphonylamino)ethyl)phenyl)-6-(3-pyridyl)hex-5-enoic acid

시약·촉매·용매 2

HCID 5963Benzyltrimethylammonium chloride촉매HCID 14798Sodium Hydroxide용매

실험 절차

2.0 g of 6-(4-(2-(4-chlorobenzenesulphonylamino)ethyl)-phenyl)-6-(3-pyridyl)hex-5-enoic acid are stirred overnight in 10 ml of 4N sodium hydroxide solution, 100 ml of methylene chloride, 80 mg of benzyl trimethylammonium chloride and 0.85 g of methyl iodide. Then the organic phase is separated off and the aqueous phase is acidified to pH 5. The product precipitated is separated off and taken up in methylene chloride, dried and evaporated down. Finally, the residue is chromatographed with ethylene chloride/methanol (97:3) over a silica gel column.

후처리

  1. customThen the organic phase is separated off
  2. customThe product precipitated
  3. customis separated off
  4. customdried
  5. customevaporated down
  6. customFinally, the residue is chromatographed with ethylene chloride/methanol (97:3) over a silica gel column

출처 및 근거

ORD 기록
ord-5193915b0bde4c429b5f8ef4d1e5471f
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05681961

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