Miconazole → Fludazonium chloride

HRID 1730210

反応式

HRID 1730210 の反応式
[Cl:1][C:2]1[CH:24]=[C:23]([Cl:25])[CH:22]=[CH:21][C:3]=1[CH:4]([O:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[Cl:20])[CH2:5][N:6]1[CH:10]=[CH:9][N:8]=[CH:7]1.Cl[CH2:27][C:28]([C:30]1[CH:35]=[CH:34][C:33]([F:36])=[CH:32][CH:31]=1)=[O:29]>C(Cl)Cl>[Cl-:1].[Cl:1][C:2]1[CH:24]=[C:23]([Cl:25])[CH:22]=[CH:21][C:3]=1[CH:4]([O:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[Cl:20])[CH2:5][N+:6]1[CH:10]=[CH:9][N:8]([CH2:27][C:28](=[O:29])[C:30]2[CH:35]=[CH:34][C:33]([F:36])=[CH:32][CH:31]=2)[CH:7]=1

参加物

4

反応物 2

HCID 4189MiconazoleHCID 1202482-Chloro-4'-fluoroacetophenone

生成物 1

HCID 178521219Fludazonium chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a manner similar to that previously described, 4.2 parts of 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]-imidazole, 1.7 parts of 2-chloro-4'-fluoroacetophenone and 40 parts of methylene chloride are mixed together and stirred at reflux temperature for 15 hours. Thereafter, the solvent is evaporated under reduced pressure and the residue triturated in 4-methyl-2-pentanone. The solid is recovered by filtration and crystallized from acetonitrile to obtain a purified 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]-3-(p-fluorobenzoylmethyl)-imidazolium chloride product, mp. 181° C.

後処理

  1. temperatureat reflux temperature for 15 hours
  2. customThereafter, the solvent is evaporated under reduced pressure
  3. customthe residue triturated in 4-methyl-2-pentanone
  4. filtrationThe solid is recovered by filtration
  5. customcrystallized from acetonitrile

出典と根拠

ORDレコード
ord-e94936bb18474fdb94e445d1e546c37b
出典データセット
uspto-grants-1976_11
特許番号
US03991202

関連ノート

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