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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
ノート
印刷プレビュー

反応式

HRID 434380 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aa6266b5fb384ae5aac373f69984a715
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04396624

反応ノート

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