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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
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HRID 556721 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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4

반응물 2

HCID 311Citric AcidHCID 16035068Azd-3199

생성물 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 citrate수율 45%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-01dd431abb1747cdb77976fb9052e323
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08058294B2

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