Trifluoroacetic acid → 3-Chloro-N-cyclopentyl-N-(3-hydroxy-propyl)-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate

HRID 2268632ノート

反応式

HRID 2268632 の反応式
C(OC(=O)[N:7]([CH2:14][CH2:15][O:16][C:17]1[CH:22]=[C:21]([C:23](=[O:34])[N:24]([CH:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)[CH2:25][CH2:26][CH2:27][OH:28])[CH:20]=[C:19]([Cl:35])[CH:18]=1)[C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)(C)(C)C.[F:37][C:38]([F:43])([F:42])[C:39]([OH:41])=[O:40]>ClCCl>[F:37][C:38]([F:43])([F:42])[C:39]([OH:41])=[O:40].[Cl:35][C:19]1[CH:20]=[C:21]([CH:22]=[C:17]([O:16][CH2:15][CH2:14][NH:7][C:8]2[CH:9]=[CH:10][N:11]=[CH:12][CH:13]=2)[CH:18]=1)[C:23]([N:24]([CH:29]1[CH2:30][CH2:31][CH2:32][CH2:33]1)[CH2:25][CH2:26][CH2:27][OH:28])=[O:34]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 54299674(2-{3-Chloro-5-[cyclopentyl-(3-hydroxy-propyl)-carbamoyl]-phenoxy}-ethyl)-pyridin-4-yl-carbamic acid tert-butyl ester

生成物 1

HCID 183492073-Chloro-N-cyclopentyl-N-(3-hydroxy-propyl)-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of (2-{3-chloro-5-[cyclopentyl-(3-hydroxy-propyl)-carbamoyl]-phenoxy}-ethyl)-pyridin-4-yl-carbamic acid tertbutyl ester (0.07 g) in a mixture of dichloromethane (2 ml) and trifluoroacetic acid (2 ml) was stored at room temperature for 1 h and then concentrated under reduced pressure. The residue was subjected to preparative hplc and the title compound (0.011 g) was obtained as a colourless gum by concentration of the required fraction under reduced pressure and drying by repetitive addition of acetonitrile and concentration under reduced pressure.

後処理

  1. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-4f09d7994ffb4dd6ac239e894e655839
出典データセット
uspto-grants-2001_12
特許番号
US06326386B1

反応ノート

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