Sodium hydride → Benzyl 4-amino-3-oxopiperazine-1-carboxylate

HRID 2086229노트

반응식

HRID 2086229 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][NH:14][C:13](=[O:17])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].C1(P(C2C=CC=CC=2)(O[NH2:29])=O)C=CC=CC=1>CN(C=O)C>[NH2:29][N:14]1[CH2:15][CH2:16][N:11]([C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[O:10])[CH2:12][C:13]1=[O:17]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 736777Benzyl 3-oxopiperazine-1-carboxylateHCID 10955453O-(Diphenylphosphinyl)hydroxylamine

생성물 1

HCID 22727156Benzyl 4-amino-3-oxopiperazine-1-carboxylate수율 96.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-(Benzyloxycarbonyl)-2-piperazinone (4.685 g) was dissolved in DMF (170 ml) and combined with sodium hydride (800 mg, in oil) with cooling on ice. After stirring at room temperature for 30 minutes, O-diphenylphosphinyl hydroxylamine (4.896 g) was added and the mixture was stirred at 50° C. for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was combined with aqueous sodium bicarbonate and extracted with dichloromethane. The extract was dried and concentrated to obtain the title compound 1-amino-4-benzyloxycarbonyl-2-piperazinone (4.8 g) as a colorless oil.

후처리

  1. temperaturewith cooling on ice
  2. stirringthe mixture was stirred at 50° C. for 15 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. extractionextracted with dichloromethane
  5. customThe extract was dried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-328225b4edb24604a071d2160f817db0
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06723722B1

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