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Ethanol → HCID 19821136、化合物

HRID 1029995
ノート
印刷プレビュー

反応式

HRID 1029995 の反応式
[OH-].[Na+].C([O:6][C:7]1[CH:12]=[C:11]([NH:13][C:14](=[O:16])[CH3:15])[C:10]([O:17][CH3:18])=[CH:9][C:8]=1[CH3:19])(=O)C.C(O)C>C(O)(=O)C>[CH3:19][C:8]1[CH:9]=[C:10]([O:17][CH3:18])[C:11]([NH:13][C:14](=[O:16])[CH3:15])=[CH:12][C:7]=1[OH:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 19821145HCID 19821145、化合物

生成物 1

HCID 19821136HCID 19821136、化合物収率 75%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To 35 ml of a 0.4N aqueous solution of sodium hydroxide were added 1.70 g (7.17 mmol) of 2-methyl-4-methoxy-5-acetylaminophenyl acetate and 10 ml of ethanol. The mixture was stirred at room temperature for 10 minutes. When crystals were completely dissolved, the stirring was ceased. Then 0.3 ml of acetic acid was added and thus crystals were precipitated. The crystals were collected by filtration, purified by column chromatography (Silica Gel 60, trade name, manufactured by Merck Co., 230-400 mesh, 200 g, eluent: ethyl acetate) and recrystallized from the solvent mixture of ethyl acetate/hexane (2:1). Thus 1.05 g (5.38 mmol) of 2-methyl-4-methoxy-5-acetylaminophenol was obtained. The yield was 75%.

後処理

  1. dissolutionWhen crystals were completely dissolved
  2. customthus crystals were precipitated
  3. filtrationThe crystals were collected by filtration
  4. custompurified by column chromatography (Silica Gel 60, trade name, manufactured by Merck Co., 230-400 mesh, 200 g, eluent: ethyl acetate)
  5. customrecrystallized from the solvent mixture of ethyl acetate/hexane (2:1)

出典と根拠

ORDレコード
ord-cce48bc9446443a29a1337f064ab5680
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05104414

反応ノート

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