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

HRID 892875노트

반응식

HRID 892875 반응식
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]

참가 물질

5

반응물 3

HCID 9804-NitrophenolHCID 10868DicyclohexylcarbodiimideHCID 19893582HCID 19893582, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ce0fbb73cff5439e95bd61cd13853736
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05120738

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