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Anisole → N,N'-di-(4-chlorophenethyl)-2-(2-mercapto-3-phenylpropionylamino)malonamide

HRID 2269826
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HRID 2269826 반응식
[Cl:1][C:2]1[CH:46]=[CH:45][C:5]([CH2:6][CH2:7][NH:8][C:9](=[O:44])[CH:10]([NH:23][C:24](=[O:43])[C@@H:25]([S:33]CC2C=CC(OC)=CC=2)[CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:11]([NH:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)=[O:12])=[CH:4][CH:3]=1.C1(OC)C=CC=CC=1>ClCCl.C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[Cl:1][C:2]1[CH:46]=[CH:45][C:5]([CH2:6][CH2:7][NH:8][C:9](=[O:44])[CH:10]([NH:23][C:24](=[O:43])[CH:25]([SH:33])[CH2:26][C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:11]([NH:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)=[O:12])=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 7519AnisoleHCID 20713101N,N'-di-(4-chlorophenethyl)-2-((S)-2-(p-methoxybenzylmercapto)-3-phenylpropionylamino)malonamide

생성물 1

HCID 18348091N,N'-di-(4-chlorophenethyl)-2-(2-mercapto-3-phenylpropionylamino)malonamide수율 80%

시약·촉매·용매 2

HCID 15337Mercuric acetate촉매HCID 6344Dichloromethane
용매

실험 절차

Combine of N,N′-di-(4-chlorophenethyl)-2-((S)-2-(p-methoxybenzylmercapto)-3-phenylpropionylamino)malonamide (0.29 g, 0.43 mmol), mercury (II) acetate (0.171 g, 0.54 mmol), and anisole (0.47 mL) in dichloromethane (10 mL). Cool in an ice bath and degas by repeatedly applying vacuum and filling the vessel with nitrogen. Add trifluoroacetic acid (4 mL). After 3 hours, purge with hydrogen sulfide (gas) for about 10 minutes. Filter and evaporate in vacuo to give a residue. Triturate the residue with diethyl ether to give the title compound as a solid (80%).

후처리

  1. temperatureCool in an ice bath
  2. customdegas
  3. custompurge with hydrogen sulfide (gas) for about 10 minutes
  4. filtrationFilter
  5. customevaporate in vacuo
  6. customto give a residue
  7. customTriturate the residue with diethyl ether

출처 및 근거

ORD 기록
ord-29e1b160da1e45e6972254ea4e4f50a5
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06329550B1

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