4-Aminophenol → 2,4-Diacetoxy-N-[3-[(4-hydroxyphenyl)amino]-3-oxopropyl]-3,3-dimethylbutanamide

HRID 892879ノート

反応式

HRID 892879 の反応式
C(N=C=NCCCN(C)C)C.[C:12]([O:15][CH:16]([C:25]([CH3:32])([CH3:31])[CH2:26][O:27][C:28](=[O:30])[CH3:29])[C:17]([NH:19][CH2:20][CH2:21][C:22]([OH:24])=O)=[O:18])(=[O:14])[CH3:13].[CH:33]1[C:38]([NH2:39])=[CH:37][CH:36]=[C:35]([OH:40])[CH:34]=1>C(Cl)Cl>[C:12]([O:15][CH:16]([C:25]([CH3:32])([CH3:31])[CH2:26][O:27][C:28](=[O:30])[CH3:29])[C:17]([NH:19][CH2:20][CH2:21][C:22]([NH:39][C:38]1[CH:33]=[CH:34][C:35]([OH:40])=[CH:36][CH:37]=1)=[O:24])=[O:18])(=[O:14])[CH3:13]

参加物

5

反応物 3

HCID 4034-AminophenolHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 19893582HCID 19893582、化合物

生成物 1

HCID 198936262,4-Diacetoxy-N-[3-[(4-hydroxyphenyl)amino]-3-oxopropyl]-3,3-dimethylbutanamide収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide (2.30 g) was added to a solution of 3.03 g of 3-[N-(2,4-diacetoxy-3,3-dimethyl-1-oxobutyl)amino]propionic acid and 2.18 g of p-aminophenol in 50 ml of methylene chloride, and the mixture was stirred for one night. After completion of the reaction, the reaction mixture was washed with water, and dried over anhydrous sodium sulfate. After removing the solvent by evaporation, the residue obtained was purified by silica gel column chromatography to obtain 1.92 g of the objective compound was obtained as a residue (yield: 50%).

後処理

  1. customAfter completion of the reaction
  2. washthe reaction mixture was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customAfter removing the solvent
  5. customby evaporation
  6. customthe residue obtained
  7. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-29ebae54edf34cfdbcc7eb7763d0fa8a
出典データセット
uspto-grants-1992_06
特許番号
US05120738

反応ノート

読み込み中…