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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
ノート
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反応式

HRID 2397527 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 9321HydrazineHCID 12282573HCID 12282573、化合物

生成物 1

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

実験手順

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.

後処理

  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
  • 出典と根拠

    ORDレコード
    ord-de2dc72c45214ed28f82e717993fa7b3
    出典データセット
    uspto-grants-1977_05
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04022766

    反応ノート

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