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 2081096Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2081096
[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]

Komponenten

4

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 24810239HCID 24810239, Verbindung

Produkt 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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

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%).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-bf7c645fb7fd4a84baa4983e314a66c4
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07932390B2

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