Tetrahydrofuran → N-[(Dimethylamino)methyl]-N-(4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2,4-dichlorobenzamide

HRID 1740027노트

반응식

HRID 1740027 반응식
[H-].[Na+].[CH:3]1[CH:4]=[CH:5][N:6]2[CH2:12][C:11]3[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=3[N:9]([C:17]([C:19]3[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:35])[C:27]4[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][C:28]=4[Cl:34])=[CH:21][CH:20]=3)=[O:18])[CH2:8][C:7]=12.[I-].C[CH:38]=[N+:39]=[CH:40]C.O1CCC[CH2:43]1>C(OCC)C>[CH3:38][N:39]([CH2:40][N:25]([C:22]1[CH:21]=[CH:20][C:19]([C:17]([N:9]2[C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[CH2:12][N:6]3[CH:5]=[CH:4][CH:3]=[C:7]3[CH2:8]2)=[O:18])=[CH:24][CH:23]=1)[C:26](=[O:35])[C:27]1[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][C:28]=1[Cl:34])[CH3:43]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 9826254N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)-phenyl]2,4-dichlorobenzamideHCID 21892197N,N-dimethylmethyleneammoniumiodide

생성물 1

HCID 70057901N-[(Dimethylamino)methyl]-N-(4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2,4-dichlorobenzamide

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a suspension under argon of 0.072 g of sodium hydride (60% in oil) in 10 ml of tetrahydrofuran is added 0.71 g of N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2,4-dichlorobenzamide and the mixture stirred at room temperature for 1 hour. To the mixture is added N,N-dimethylmethyleneammonium iodide and the mixture stirred 20 hours. The mixture is diluted with diethyl ether (30 ml), filtered and the filtrate concentrated under vacuum. The residue is triturated with hexane to give 0.76 g of white solid, m.p. 126-129° C.

후처리

  1. stirringthe mixture stirred 20 hours
  2. filtrationfiltered
  3. concentrationthe filtrate concentrated under vacuum
  4. customThe residue is triturated with hexane

출처 및 근거

ORD 기록
ord-f67d8be9ba7c43c3965ecea109649968
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05968930

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