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Hydrazine → Pyrrolo(1,2-a)(1,4)diazepine

HRID 439982
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HRID 439982 반응식
[N+](C1C=CC(C([N:10]2[C:16]3OC=C[C:15]=3[CH2:14][N:13]3[CH:20]=[CH:21][CH:22]=[C:12]3[CH2:11]2)=O)=CC=1)([O-])=O.NN>C(O)C.[Pd]>[CH:11]1[C:12]2[N:13]([CH:20]=[CH:21][CH:22]=2)[CH2:14][CH:15]=[CH:16][N:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 9321HydrazineHCID 218370989,10-dihydro-10-(4-nitrobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine

생성물 1

HCID 45087533Pyrrolo(1,2-a)(1,4)diazepine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

To a solution of i mmol of 9,10-dihydro-10-(4-nitrobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]-diazepine in 20 ml of ethyl alcohol is added 0.2 g of 10% Pd/C and 2.5 mmol of hydrazine followed by stirring and heating under reflux for 3 hours. The room temperature reaction mixture is filtered through diatomaceous earth and the filtrate concentrated in vacuo. The residue is dissolved in methylene chloride and passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated in vacuo to give the desired product which is purified by flash chromatography on silica gel to give the desired product as a solid.

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후처리

  1. temperatureheating
  2. temperatureunder reflux for 3 hours
  3. customThe room temperature reaction mixture
  4. filtrationis filtered through diatomaceous earth
  5. concentrationthe filtrate concentrated in vacuo
  6. dissolutionThe residue is dissolved in methylene chloride
  7. concentrationThe filtrate is concentrated in vacuo

출처 및 근거

ORD 기록
ord-4f303ab7db724eb395e74822a1956802
출처 데이터셋
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05516774

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