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Water → HCID 10135367, 화합물

HRID 2307333
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HRID 2307333 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 178519422HCID 178519422, 화합물

생성물 1

HCID 10135367HCID 10135367, 화합물수율 82.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2c61790987b0487d8100a0c15dd103cb
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06831079B1

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