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1-((6-Chloronaphthalen-2-yl)sulfonyl)piperazine → 1-(6-Chloronaphthalene-2-sulfonyl)-4-(6-chloropyridazin-3-ylcarbonyl)piperazine

HRID 1372883
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인쇄 미리보기

반응식

HRID 1372883 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)(=[O:14])=[O:13])[CH:6]=[CH:5]2.[Cl:21][C:22]1[N:27]=[N:26][C:25]([C:28](Cl)=[O:29])=[CH:24][CH:23]=1>C(Cl)Cl.N1C=CC=CC=1.C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]1[CH2:16][CH2:17][N:18]([C:28]([C:25]3[N:26]=[N:27][C:22]([Cl:21])=[CH:23][CH:24]=3)=[O:29])[CH2:19][CH2:20]1)(=[O:13])=[O:14])[CH:6]=[CH:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 113588251-((6-Chloronaphthalen-2-yl)sulfonyl)piperazineHCID 217811856-Chloropyridazine-3-carbonyl chloride

생성물 1

HCID 210726741-(6-Chloronaphthalene-2-sulfonyl)-4-(6-chloropyridazin-3-ylcarbonyl)piperazine수율 76.4%

시약·촉매·용매 3

HCID 1049Pyridine용매2회HCID 6212Chloroform용매
HCID 6344
Dichloromethane
용매

실험 절차

To a solution of 1-(6-chloronaphthalen-2-ylsulfonyl)-piperazine (0.450 g, 1.45 mmol) in methylene chloride (100 mL) and pyridine (0.154 mL) was added dropwise 6-chloropyridazine-3-carbonyl chloride (1.74 mmol). After the addition of the acid chloride, pyridine (0.154 mL) was added, and the reaction mixture was stirred overnight. The reaction mixture was diluted with chloroform (500 mL), washed with saturated sodium bicarbonate (200 mL), water (200 mL),and brine and dried over MgSO4. After filtration and evaporation of the solvent, trituration of the residue with ethyl acetate and filtration gave the product as a white powder (0.5 g, 76%)

후처리

  1. additionwas added
  2. washwashed with saturated sodium bicarbonate (200 mL), water (200 mL),and brine
  3. dry with materialdried over MgSO4
  4. filtrationAfter filtration and evaporation of the solvent, trituration of the residue
  5. filtrationwith ethyl acetate and filtration

출처 및 근거

ORD 기록
ord-c2732702d5f64975b55e9c81357befb9
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07160878B2

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