Miconazole → Fludazonium chloride

HRID 1730210

반응식

HRID 1730210 반응식
[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

참가 물질

4

반응물 2

HCID 4189MiconazoleHCID 1202482-Chloro-4'-fluoroacetophenone

생성물 1

HCID 178521219Fludazonium chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e94936bb18474fdb94e445d1e546c37b
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03991202

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