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

HRID 1490381

反応式

HRID 1490381 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 5963Benzyltrimethylammonium chloride触媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5193915b0bde4c429b5f8ef4d1e5471f
出典データセット
uspto-grants-1997_10
特許番号
US05681961

関連ノート

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