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Water → HCID 10135367、化合物

HRID 2307333
ノート
印刷プレビュー

反応式

HRID 2307333 の反応式
[NH:1]1[CH:5]=[CH:4][C:3]([C:6]2[CH:11]=[CH:10][C:9]([C:12]([N:14]3[C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=4[CH2:18][N:17]4[CH:25]=[CH:26][CH:27]=[C:16]4[CH2:15]3)=[O:13])=[CH:8][CH:7]=2)=[N:2]1.[C:28](OC(=O)C)(=[O:30])[CH3:29].O>N1C=CC=CC=1>[CH:27]1[CH:26]=[CH:25][N:17]2[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:14]([C:12]([C:9]3[CH:10]=[CH:11][C:6]([C:3]4[CH:4]=[CH:5][N:1]([C:28](=[O:30])[CH3:29])[N:2]=4)=[CH:7][CH:8]=3)=[O:13])[CH2:15][C:16]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 178519422HCID 178519422、化合物

生成物 1

HCID 10135367HCID 10135367、化合物収率 82.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of [4-(1H-pyrazol-3-yl)-phenyl]-(5H,11H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-methanone (0.50 g) in dry pyridine (10 ml) was added acetic anhydride (0.20 g). After stirring at room temperature for 18 hours the reaction mixture was poured into water and the precipitate was collected by filtration. The crude product was dissolved in dichloromethane and dried over anhydrous sodium sulfate. This solution was filtered through a short column of hydrous sodium magnesium silicate, eluting with several additional volumes of dichloromethane. The eluant was concentrated on a hot plate with the gradual addition of hexane until crystallization occurred. After cooling, the crystals were collected by filtration to yield the title compound (0.46 g), m.p. 192-194° C.

後処理

  1. filtrationthe precipitate was collected by filtration
  2. dissolutionThe crude product was dissolved in dichloromethane
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThis solution was filtered through a short column of hydrous sodium magnesium silicate
  5. washeluting with several additional volumes of dichloromethane
  6. concentrationThe eluant was concentrated on a hot plate with the gradual addition of hexane until crystallization
  7. temperatureAfter cooling
  8. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-2c61790987b0487d8100a0c15dd103cb
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06831079B1

反応ノート

読み込み中…

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