p-Toluenesulfonic acid monohydrate → 4-Amino-3-{5-[1-(4-chloro-benzyl)-1h-[1,2,3]triazol-4-yl]-2-methyl-phenoxymethyl}-thieno[3,2-c]pyridine-7-carboxylic acid (2-hydroxy-ethyl)-amide toluene-4-sulfonic acid salt

HRID 2081096ノート

反応式

HRID 2081096 の反応式
[OH:1][CH2:2][CH2:3][NH:4][C:5]([C:7]1[C:8]2[S:16][CH:15]=[C:14]([CH2:17][O:18][C:19]3[CH:24]=[C:23]([C:25]4[N:26]=[N:27][N:28]([CH2:30][C:31]5[CH:36]=[CH:35][C:34]([Cl:37])=[CH:33][CH:32]=5)[CH:29]=4)[CH:22]=[CH:21][C:20]=3[CH3:38])[C:9]=2[C:10]([NH2:13])=[N:11][CH:12]=1)=[O:6].O.[C:40]1([CH3:50])[CH:45]=[CH:44][C:43]([S:46]([OH:49])(=[O:48])=[O:47])=[CH:42][CH:41]=1>CO>[C:40]1([CH3:50])[CH:41]=[CH:42][C:43]([S:46]([OH:49])(=[O:47])=[O:48])=[CH:44][CH:45]=1.[OH:1][CH2:2][CH2:3][NH:4][C:5]([C:7]1[C:8]2[S:16][CH:15]=[C:14]([CH2:17][O:18][C:19]3[CH:24]=[C:23]([C:25]4[N:26]=[N:27][N:28]([CH2:30][C:31]5[CH:32]=[CH:33][C:34]([Cl:37])=[CH:35][CH:36]=5)[CH:29]=4)[CH:22]=[CH:21][C:20]=3[CH3:38])[C:9]=2[C:10]([NH2:13])=[N:11][CH:12]=1)=[O:6]

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 24810239HCID 24810239、化合物

生成物 1

HCID 248102404-Amino-3-{5-[1-(4-chloro-benzyl)-1h-[1,2,3]triazol-4-yl]-2-methyl-phenoxymethyl}-thieno[3,2-c]pyridine-7-carboxylic acid (2-hydroxy-ethyl)-amide toluene-4-sulfonic acid salt

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To solution of 4-amino-3-{5-[1-(4-chloro-benzyl)-1H-[1,2,3]triazol-4-yl]-2-methyl-phenoxymethyl}-thieno[3,2-c]pyridine-7-carboxylic acid (2-hydroxy-ethyl)-amide (0.159 g, 0.29 mmol) (from Example 37 supra) in methanol (10 mL) was treated with toluene-4-sulfonic acid hydrate (61.0 mg, 0.319 mmol) and heated at room temperature for 40 minutes. The solution was concentrated. The residue washed with diethyl ether, dissolved in water and lyophilized to 4-amino-3-{5-[1-(4-chloro-benzyl)-1H-[1,2,3]triazol-4-yl]-2-methyl-phenoxymethyl}-thieno[3,2-c]pyridine-7-carboxylic acid (2-hydroxy-ethyl)-amide 1.5 toluene-4-sulfonic acid salt. (Yield 0.21 g, 100%).

後処理

  1. concentrationThe solution was concentrated
  2. washThe residue washed with diethyl ether
  3. dissolutiondissolved in water

出典と根拠

ORDレコード
ord-bf7c645fb7fd4a84baa4983e314a66c4
出典データセット
uspto-grants-2011_04
特許番号
US07932390B2

反応ノート

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