4-Nitrophenol → 4-Nitropheny 3-[N-(2,4-diacetoxy 3,3-dimethyl-1-oxobutyl)amino]propionate

HRID 892875ノート

反応式

HRID 892875 の反応式
C1(N=C=NC2CCCCC2)CCCCC1.[C:16]([O:19][CH:20]([C:29]([CH3:36])([CH3:35])[CH2:30][O:31][C:32](=[O:34])[CH3:33])[C:21]([NH:23][CH2:24][CH2:25][C:26]([OH:28])=[O:27])=[O:22])(=[O:18])[CH3:17].[CH:37]1[C:42]([N+:43]([O-:45])=[O:44])=[CH:41][CH:40]=[C:39](O)[CH:38]=1>O1CCCC1>[C:16]([O:19][CH:20]([C:29]([CH3:36])([CH3:35])[CH2:30][O:31][C:32](=[O:34])[CH3:33])[C:21]([NH:23][CH2:24][CH2:25][C:26]([O:28][C:39]1[CH:38]=[CH:37][C:42]([N+:43]([O-:45])=[O:44])=[CH:41][CH:40]=1)=[O:27])=[O:22])(=[O:18])[CH3:17]

参加物

5

反応物 3

HCID 9804-NitrophenolHCID 10868DicyclohexylcarbodiimideHCID 19893582HCID 19893582、化合物

生成物 1

HCID 198935384-Nitropheny 3-[N-(2,4-diacetoxy 3,3-dimethyl-1-oxobutyl)amino]propionate収率 32.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Dicyclohexylcarbodiimide (15.5 g) was added to a solution of 22.6 g of 3-[N-(2,4-diacetoxy-3,3-dimethyl-1-oxobutyl)amino]propionic acid and 10.4 g of p-nitrophenol in 500 ml of tetrahydrofuran, and the mixture was stired for one night. After completion of the reaction, insoluble matter was removed and the solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate. The resulting solution was washed with saturated aqueous sodium bicarbonate solution, with water and then with saturated saline, and dried over anhydrous sodium sulfate. After removing the solvent by evaporation, 10.2 g of the objectived compound was obtained as a residue (yield: 32%).

後処理

  1. waitthe mixture was stired for one night
  2. customAfter completion of the reaction, insoluble matter
  3. customwas removed
  4. distillationthe solvent was distilled off under reduced pressure
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washThe resulting solution was washed with saturated aqueous sodium bicarbonate solution, with water
  7. dry with materialwith saturated saline, and dried over anhydrous sodium sulfate
  8. customAfter removing the solvent
  9. customby evaporation

出典と根拠

ORDレコード
ord-ce0fbb73cff5439e95bd61cd13853736
出典データセット
uspto-grants-1992_06
特許番号
US05120738

反応ノート

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