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Dimethylformamide → 2-(3-Chloro-biphenyl-4-yloxy)-n-[3-chloro-4-(2-diethylamino-ethoxy)-phenyl]-acetamide

HRID 898558
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HRID 898558 반응식
C(=O)([O-])[O-].[K+].[K+].Br.Br[CH2:9][C:10]([NH:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])=[C:15]([Cl:27])[CH:14]=1)=[O:11].[Cl:28][C:29]1[CH:30]=[C:31]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:32]=[CH:33][C:34]=1[OH:35].CN(C=O)C>ClCCl>[Cl:28][C:29]1[CH:30]=[C:31]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:32]=[CH:33][C:34]=1[O:35][CH2:9][C:10]([NH:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])=[C:15]([Cl:27])[CH:14]=1)=[O:11]
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참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 70742-Chloro-4-PhenylphenolHCID 11430Potassium CarbonateHCID 688779532-Bromo-n-[3-chloro-4-(2-diethylamino-ethoxy)-phenyl]-acetamide-hydrobromide

생성물 1

HCID 103453352-(3-Chloro-biphenyl-4-yloxy)-n-[3-chloro-4-(2-diethylamino-ethoxy)-phenyl]-acetamide

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

65 mg (0.47 mmol) of potassium carbonate was added to a solution of 70 mg (0.159 mmol) of 2-bromo-N-[3-chloro-4-(2-diethylamino-ethoxy)-phenyl]-acetamide-hydrobromide (intermediate product Z1c) and 64 mg (0.314 mmol) of 3-chloro-biphenyl-4-ol in 1 mL of abs. DMF and the mixture was stirred for 1 hour at 40° C. and for 15 hours at RT. The reaction mixture was diluted with dichloromethane, the org. phase was washed with sat. aqueous sodium bicarbonate solution and water and dried over magnesium sulphate. Column chromatography (silica gel, dichloromethane/MeOH 9:1) yielded the product.

후처리

  1. washphase was washed with sat. aqueous sodium bicarbonate solution and water
  2. dry with materialdried over magnesium sulphate
  3. customColumn chromatography (silica gel, dichloromethane/MeOH 9:1) yielded the product

출처 및 근거

ORD 기록
ord-8ca1535cfe144253bdfececabfc75dec
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07351719B2

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