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Citric Acid → N-[2-(diethylamino)ethyl]-N-(2-{[2-(4-hydroxy-2-oxo-2,3-dihydro-1,3-benzothiazol-7-yl)ethyl]amino}ethyl)-3-[2-(1-naphthyl)ethoxy]propanamide citrate

HRID 556721
ノート
印刷プレビュー

反応式

HRID 556721 の反応式
[C:1]([OH:13])(=[O:12])[CH2:2][C:3]([CH2:8][C:9]([OH:11])=[O:10])([C:5]([OH:7])=[O:6])[OH:4].[CH2:14]([N:16]([CH2:53][CH3:54])[CH2:17][CH2:18][N:19]([CH2:37][CH2:38][NH:39][CH2:40][CH2:41][C:42]1[C:50]2[S:49][C:48](=[O:51])[NH:47][C:46]=2[C:45]([OH:52])=[CH:44][CH:43]=1)[C:20](=[O:36])[CH2:21][CH2:22][O:23][CH2:24][CH2:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:29]=[CH:28][CH:27]=1)[CH3:15]>CO>[C:1]([OH:13])(=[O:12])[CH2:2][C:3]([CH2:8][C:9]([OH:11])=[O:10])([C:5]([OH:7])=[O:6])[OH:4].[CH2:53]([N:16]([CH2:14][CH3:15])[CH2:17][CH2:18][N:19]([CH2:37][CH2:38][NH:39][CH2:40][CH2:41][C:42]1[C:50]2[S:49][C:48](=[O:51])[NH:47][C:46]=2[C:45]([OH:52])=[CH:44][CH:43]=1)[C:20](=[O:36])[CH2:21][CH2:22][O:23][CH2:24][CH2:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:29]=[CH:28][CH:27]=1)[CH3:54]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 311Citric AcidHCID 16035068Azd-3199

生成物 1

HCID 66992113N-[2-(diethylamino)ethyl]-N-(2-{[2-(4-hydroxy-2-oxo-2,3-dihydro-1,3-benzothiazol-7-yl)ethyl]amino}ethyl)-3-[2-(1-naphthyl)ethoxy]propanamide citrate収率 45%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

Citric Acid (248.96 mg) was added to a solution of N-[2-(diethylamino)ethyl]-N-(2-{[2-(4-hydroxy-2-oxo-2,3-dihydro-1,3-benzothiazol-7-yl)ethyl]amino}ethyl)-3-[2-(1-naphthyl)ethoxy]propanamide (0.5 g) in methanol (5 mL). Immediately, the clear solution became opaque and orange oil settled out. This mixture was heated at an external temp of 60° C. forming a clear solution, which was then allowed to cool to room temperature and stirred for 48 h. The resulting precipitate was collected by filtration and washed with methanol (1 mL) and diethyl ether (1 mL). The solid was then dried in vacuo at room temperature for 4 h to give the title compound (0.3 g).

後処理

  1. customforming a clear solution, which
  2. temperatureto cool to room temperature
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with methanol (1 mL) and diethyl ether (1 mL)
  5. customThe solid was then dried in vacuo at room temperature for 4 h

出典と根拠

ORDレコード
ord-01dd431abb1747cdb77976fb9052e323
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058294B2

反応ノート

読み込み中…

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