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1H-1,2,4-Triazole → 1-((6-Chloropyridin-2-yl)oxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one

HRID 434380
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HRID 434380 반응식
ClC(Cl)C(=O)C(C)(C)C.[Cl:10][C:11]1[N:16]=[C:15]([OH:17])[CH:14]=[CH:13][CH:12]=1.N1C=NC=N1.C(=O)([O-])[O-].[K+].[K+].[N:29]1([CH:34](N2C=NC=N2)[C:35](=[O:40])[C:36]([CH3:39])([CH3:38])[CH3:37])[CH:33]=[N:32][CH:31]=[N:30]1.ClC1N=C(OC(OC2C=CC=C(Cl)N=2)C(=O)C(C)(C)C)C=CC=1>CC(C)=O>[Cl:10][C:11]1[N:16]=[C:15]([O:17][CH:34]([N:29]2[CH:33]=[N:32][CH:31]=[N:30]2)[C:35](=[O:40])[C:36]([CH3:39])([CH3:38])[CH3:37])[CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 314321,1-Dichloro-3,3-dimethyl-2-butanoneHCID 137063971,1-Bis-(1,2,4-triazol-1-yl)-3,3-dimethylbutan-2-oneHCID 204937601,1-Bis-(6-chloropyridin-2-yl-oxy)-3,3-dimethyl-butan-2-oneHCID 178516025CID 5284509

생성물 1

HCID 20493724
1-((6-Chloropyridin-2-yl)oxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

33.8 g (0.2 mol) of 1,1-dichloro-3,3-dimethyl-butan-2-one, 26 g (0.2 mol) of 6-chloro-2-hydroxy-pyridine, 21 g (0.3 mol) of 1,2,4-triazole and 56 g (0.4 mol) of potassium carbonate were heated under reflux in 250 ml of acetone for 12 hours, while stirring. Thereafter, the mixture was allowed to cool, the salt which had precipitated was filtered off and the filtrate was concentrated in vacuo. Isopropanol was added to the oily residue, it being possible to isolate successively three crystal fractions. The first two contained mainly 1,1-bis-(1,2,4-triazol-1-yl)-3,3-dimethylbutan-2-one of melting point 157°-158° C. and 1,1-bis-(6-chloropyridin-2-yl-oxy)-3,3-dimethyl-butan-2-one of melting point 102°-104° C. 4 g of 1-(6-chloropyridin-2-yl-oxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 102° C. were obtained from the third fraction.

후처리

  1. temperatureto cool
  2. customthe salt which had precipitated
  3. filtrationwas filtered off
  4. concentrationthe filtrate was concentrated in vacuo
  5. additionIsopropanol was added to the oily residue, it
  6. customto isolate successively three crystal fractions

출처 및 근거

ORD 기록
ord-aa6266b5fb384ae5aac373f69984a715
출처 데이터셋
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04396624

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