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Water → HCID 44477248, 화합물

HRID 2361672
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HRID 2361672 반응식
[N:1]([CH:4]1[CH2:7][N:6]([C:8]([N:10]2[CH2:16][CH2:15][CH2:14][N:13]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:12][CH2:11]2)=[O:9])[CH2:5]1)=[N+]=[N-].O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>C1COCC1>[CH:17]1([N:13]2[CH2:14][CH2:15][CH2:16][N:10]([C:8]([N:6]3[CH2:5][CH:4]([NH2:1])[CH2:7]3)=[O:9])[CH2:11][CH2:12]2)[CH2:20][CH2:19][CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 58243397HCID 58243397, 화합물

생성물 1

HCID 44477248HCID 44477248, 화합물수율 40.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1-[(3-azidoazetidin-1-yl)carbonyl]-4-cyclobutyl-1,4-diazepane (140 mg, 0.50 mmol), was dissolved in THF (5 ml) and water (0.28 ml, 5 mmol) was added. PPh3 was then added as a solid and the reaction was stirred for 16 hours giving a clear solution. The reaction was concentrated in vacuo and purified by FCC (DCM/MeOH/MH3 gradient, 95:5:1 to 70:30:1) to provide the title compound as pale yellow solid (51 mg, 40%).

후처리

  1. customgiving a clear solution
  2. concentrationThe reaction was concentrated in vacuo
  3. custompurified by FCC (DCM/MeOH/MH3 gradient, 95:5:1 to 70:30:1)

출처 및 근거

ORD 기록
ord-98106b405e86433587e6fcc35adaa258
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691804B2

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