Potassium Carbonate → 1-(4-Chlorobenzoyl)-1-(3-chloro-1,2,4-triazol-1-yl)-cyclopropane

HRID 893627ノート

反応式

HRID 893627 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[N:12]=[CH:11][NH:10][N:9]=1.Br[CH:14]([CH2:24][CH2:25]Cl)[C:15]([C:17]1[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=1)=[O:16]>CC(C)=O>[Cl:23][C:20]1[CH:21]=[CH:22][C:17]([C:15]([C:14]2([N:10]3[CH:11]=[N:12][C:8]([Cl:7])=[N:9]3)[CH2:25][CH2:24]2)=[O:16])=[CH:18][CH:19]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 1071672-Bromo-4-chloro-1-(4-chlorophenyl)butan-1-oneHCID 178478410HCID 178478410、化合物

生成物 1

HCID 146972271-(4-Chlorobenzoyl)-1-(3-chloro-1,2,4-triazol-1-yl)-cyclopropane収率 90%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

34 g (246 mmol) of potassium carbonate and 35 g (338 mmol) of 3-chloro-1,2,4-triazole are initially introduced into 130 ml of acetone under reflux and 50 g (169 mol) of 2-bromo-4-chloro-1-(4-chlorophenyl)-butan-1-one in 60 ml of acetone are added dropwise. The mixture is boiled under reflux for 8 hours, the solution is filtered off with suction from the residue and the solvent is stripped off in vacuo. The residue is taken up in ethyl acetate, washed with water and dried over sodium sulphate, and the solvent is evaporated. Chromatography on silica gel (eluent: dichloromethane) gives 42.9 g of the title compound (90% of theory) of m.p. 85° C.

後処理

  1. temperatureunder reflux
  2. temperatureunder reflux for 8 hours
  3. filtrationthe solution is filtered off with suction from the residue
  4. washwashed with water
  5. dry with materialdried over sodium sulphate
  6. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-ca0768b7f1a34bbbb62ba7fdc517292f
出典データセット
uspto-grants-1992_06
特許番号
US05126359

反応ノート

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