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Dimethyl Sulfoxide → 10-[(2'-Methoxy-1,1'-biphenyl-4-YL)carbonyl]-N-[(2-phenoxypyridin-3-YL)methyl]-10,11-dihydro-5H-pyrrolo[2,1-C][1,4]benzodiazepine-3-carboxamide

HRID 2244206
ノート
印刷プレビュー

反応式

HRID 2244206 の反応式
ClC(Cl)(Cl)[C:3]([C:5]1[N:14]2[C:8]([CH2:9][N:10]([C:19]([C:21]3[CH:26]=[CH:25][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[O:33][CH3:34])=[CH:23][CH:22]=3)=[O:20])[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13]2)=[CH:7][CH:6]=1)=[O:4].[Cl-].[O:38]([C:45]1[C:50]([CH2:51][NH3+:52])=[CH:49][CH:48]=[CH:47][N:46]=1)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1.C(N(CC)CC)C.CS(C)=O>C(#N)C>[CH3:34][O:33][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=1[C:24]1[CH:23]=[CH:22][C:21]([C:19]([N:10]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13][N:14]3[C:5]([C:3]([NH:52][CH2:51][C:50]4[C:45]([O:38][C:39]5[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=5)=[N:46][CH:47]=[CH:48][CH:49]=4)=[O:4])=[CH:6][CH:7]=[C:8]3[CH2:9]2)=[O:20])=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 160384072,2,2-trichloro-1-{10-[(2'-methoxy-1,1'-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanoneHCID 866096892-Phenoxy-pyridin-3-ylmethyl-ammonium chloride

生成物 1

HCID 1595308210-[(2'-Methoxy-1,1'-biphenyl-4-YL)carbonyl]-N-[(2-phenoxypyridin-3-YL)methyl]-10,11-dihydro-5H-pyrrolo[2,1-C][1,4]benzodiazepine-3-carboxamide
収率 26.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The title compound was prepared according to the procedure of Example 6, Step D, from 2,2,2-trichloro-1-{10-[(2′-methoxy-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone (0.20 g, 0.379 mmol), 2-phenoxy-pyridin-3-ylmethyl-ammonium chloride (0.192 g, 0.78 mmol), triethylamine (0.112 g, 0.8 mmol), dimethylsulfoxide (0.131 mL, 1.85 mmol), and acetonitrile (5 mL). The crude material was purified by hplc using the following conditions: solvent system, 65:35 acetonitrile:water (0.1% trifluoroacetic acid); Primesphere 10 C18, 250 by 50 mm column; flow rate 100 mL/min) to provide the title compound (0.062 g) as a white solid.

後処理

  1. customThe title compound was prepared
  2. customThe crude material was purified by hplc

出典と根拠

ORDレコード
ord-cf7ba76a442340059aa3a59af4ea7cde
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07678787B2

反応ノート

読み込み中…

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