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Sodium hydride → HCID 22727141, 화합물

HRID 2086245
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인쇄 미리보기

반응식

HRID 2086245 반응식
[CH3:1][CH:2]1[NH:7][C:6](=[O:8])[CH2:5][N:4]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:3]1.[H-].[Na+].C1(P(C2C=CC=CC=2)(O[NH2:27])=O)C=CC=CC=1>CN(C=O)C>[NH2:27][N:7]1[C:6](=[O:8])[CH2:5][N:4]([C:9]([O:11][C:12]([CH3:14])([CH3:13])[CH3:15])=[O:10])[CH2:3][CH:2]1[CH3:1]
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 10955453O-(Diphenylphosphinyl)hydroxylamineHCID 22727032Tert-butyl 3-methyl-5-oxopiperazine-1-carboxylate

생성물 1

HCID 22727141HCID 22727141, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

tert-Butyl 3-methyl-5-oxo-1-piperazinecarboxylate (1.1 g) was dissolved in DMF (20 ml) and treated with sodium hydride (0.25 g, in oil) with cooling on ice. After stirring at 50° C. for 1 hour, O-diphenylphosphinyl hydroxylamine (1.3 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 tert-butyl 4-amino-3-methyl-5-oxo-1-piperazinecarboxylate as a yellow 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-949b143a25dd4de0a691795ea3f75acd
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06723722B1

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