Ethanol → N-hydroxy-2-[[4-methoxybenzenesulfonyl](2-quinolinylmethyl)amino]acetamide

HRID 2209702

反応式

HRID 2209702 の反応式
C([O:5][NH:6][C:7](=[O:32])[CH2:8][N:9]([S:21]([C:24]1[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[CH:26][CH:25]=1)(=[O:23])=[O:22])[CH2:10][C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]=1)(C)(C)C.C(O)C>C(Cl)Cl>[OH:5][NH:6][C:7](=[O:32])[CH2:8][N:9]([S:21]([C:24]1[CH:25]=[CH:26][C:27]([O:30][CH3:31])=[CH:28][CH:29]=1)(=[O:23])=[O:22])[CH2:10][C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]=1

参加物

4

反応物 2

HCID 702EthanolHCID 22907171N-(t-Butyloxy)-2-[[4-methoxybenzenesulfonyl](2-quinolinylmethyl)amino]acetamide

生成物 1

HCID 22907131N-hydroxy-2-[[4-methoxybenzenesulfonyl](2-quinolinylmethyl)amino]acetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-(t-Butyloxy)-2-[[4-methoxybenzenesulfonyl](2-quinolinylmethyl)amino]acetamide (1.15g, 2.42 mmol) is dissolved in methylene chloride (30.0 mL) and ethanol (0.20 mL) in a glass sealed tube. Hydrochloric acid gas (from a lecture bottle) is bubbled through the solution for 20 minutes, and then the tube is sealed and stands at room temperature overnight. The next day, additional hydrochloric acid gas is bubbled through the solution for 20 minutes, more ethanol (0.20 mL) is added, and then the tube is sealed and stands at room temperature for two days. After that time, the solvent is removed. The product is purified by silca gel chromatography (5% to 15% methanol/methylene chloride with ~1% ammonium hydroxide) to give N-hydroxy-2-[[4-methoxybenzenesulfonyl](2-quinolinylmethyl)amino]acetamide, m.p. 177°-178° C.

後処理

  1. customHydrochloric acid gas (from a lecture bottle) is bubbled through the solution for 20 minutes
  2. customthe tube is sealed
  3. customThe next day, additional hydrochloric acid gas is bubbled through the solution for 20 minutes
  4. additionmore ethanol (0.20 mL) is added
  5. customthe tube is sealed
  6. waitstands at room temperature for two days
  7. customAfter that time, the solvent is removed
  8. customThe product is purified by silca gel chromatography (5% to 15% methanol/methylene chloride with ~1% ammonium hydroxide)

出典と根拠

ORDレコード
ord-ba3ba135438944c0838d0d7c73b30304
出典データセット
uspto-grants-1995_10
特許番号
US05455258

関連ノート

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