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Hydrazine → Pyrrolo(3,4-e)(1,4)diazepin-2(1H)-one, 3,7-dihydro-5,8-diphenyl-6-methyl-

HRID 2397527
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HRID 2397527 반응식
NN.C([C:11]1[C:15]([NH:16][C:17](=[O:30])[CH2:18][N:19]2C(=O)[C:22]3=[CH:25][CH:26]=[CH:27][CH:28]=[C:21]3[C:20]2=O)=[C:14](C2C=CC=CC=2)[NH:13][C:12]=1[CH3:37])(=O)C1C=CC=CC=1>>[C:21]1([C:20]2[C:11]3[C:15](=[C:14]([C:21]4[CH:22]=[CH:25][CH:26]=[CH:27][CH:28]=4)[NH:13][C:12]=3[CH3:37])[NH:16][C:17](=[O:30])[CH2:18][N:19]=2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 9321HydrazineHCID 12282573HCID 12282573, 화합물

생성물 1

HCID 3044501Pyrrolo(3,4-e)(1,4)diazepin-2(1H)-one, 3,7-dihydro-5,8-diphenyl-6-methyl-

실험 절차

To a solution of 7 g. of anhydrous hydrazine in 350 ml. of methano 27.8 g. of 3-benzoyl-2-methyl-5-phenyl-4-(phthalimidoacetamido)pyrrole are added and the mixture is refluxed for one hour. The solvent is evaporated off and 150 ml. of concentrated hydrochloric acid are added to the residue. After refluxing for one hour the solid precipitated is eliminated by filtration and the filtrate is diluted with water and then alkalinized with 10% sodium hydroxide. The precipitate is crystallized twice from methanol yielding 9 g. of the title product which melts at 310°-12° C.

후처리

  1. temperaturethe mixture is refluxed for one hour
  2. customThe solvent is evaporated off
  3. additionof concentrated hydrochloric acid are added to the residue
  • temperatureAfter refluxing for one hour the solid
  • customprecipitated
  • filtrationis eliminated by filtration
  • additionthe filtrate is diluted with water
  • customThe precipitate is crystallized twice from methanol yielding 9 g
  • 출처 및 근거

    ORD 기록
    ord-de2dc72c45214ed28f82e717993fa7b3
    출처 데이터셋
    uspto-grants-1977_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04022766

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