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HCID 22008532, 화합물 → 2-(3,5-Dichloro-4-(4-chlorobenzyl)phenyl)-1,2,4-triazine-3,5(2H,4H)-dione

HRID 1604322
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HRID 1604322 반응식
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH2:6][C:7]2[C:12]([Cl:13])=[CH:11][C:10]([N:14]3[C:19](=[O:20])[NH:18][CH2:17][CH:16]=[N:15]3)=[CH:9][C:8]=2[Cl:21])=[CH:4][CH:3]=1.[Cr](Cl)([O-])(=O)=[O:25].[NH+]1C=CC=CC=1>O1CCCC1>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH2:6][C:7]2[C:12]([Cl:13])=[CH:11][C:10]([N:14]3[C:19](=[O:20])[NH:18][C:17](=[O:25])[CH:16]=[N:15]3)=[CH:9][C:8]=2[Cl:21])=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 22008532HCID 22008532, 화합물HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 150529132-(3,5-Dichloro-4-(4-chlorobenzyl)phenyl)-1,2,4-triazine-3,5(2H,4H)-dione수율 81.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In 30 ml of tetrahydrofuran was dissolved 2.6 g of 2-[4-(4-chlorobenzyl)-3,5-dichlorophenyl]-4,5-dihydro-1,2,4-triazin-3(2H)-one. To the solution was added 4.5 g of pyridinium chlorochromate. The mixture was stirred at room temperature overnight, after which the insoluble matter was filtered off. The filtrate was concentrated. The residue was purified by column chromatography (Merck Silica Gel 60; chloroform-ethanol=20:1) to provide 2.2 g of the title compound as colorless crystals, m.p. 175-176° C.

후처리

  1. filtrationafter which the insoluble matter was filtered off
  2. concentrationThe filtrate was concentrated
  3. customThe residue was purified by column chromatography (Merck Silica Gel 60; chloroform-ethanol=20:1)

출처 및 근거

ORD 기록
ord-59130b63a51944e38ee48a9f7d48ee33
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05994355

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