Miconazole → Fludazonium chloride

HRID 328639

反応式

HRID 328639 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-dichloroβ-(2,4-dichlorobenzyloxy)phenethyl]-3-(p-fluorobenzoylmethyl)imidazolium chloride product, m.p. 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-98e3ef4685bc4e8fb9ab499c88062115
出典データセット
uspto-grants-1977_04
特許番号
US04017631

関連ノート

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