Imidazole → 1-(2-chloro-4-fluorophenyl)-2-(1H-imidazol-1-yl)ethanone hydrochloride

HRID 1706904노트

반응식

HRID 1706904 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[Cl:12])=[O:4].O(CC)CC.[NH:18]1[CH:22]=[CH:21][N:20]=[CH:19]1.CN(C)C=O>O>[ClH:12].[Cl:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[C:3](=[O:4])[CH2:2][N:18]1[CH:22]=[CH:21][N:20]=[CH:19]1

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 3283Diethyl EtherHCID 6228DimethylformamideHCID 125933352-Chloro-4-fluorophenacyl bromide

생성물 1

HCID 203326301-(2-chloro-4-fluorophenyl)-2-(1H-imidazol-1-yl)ethanone hydrochloride

시약·촉매·용매 1

HCID 962Water용매

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온도
50 °C

실험 절차

To a stirred solution of 78.7 parts of 2-bromo-1-(2-chloro-4-fluorophenyl)ethanone in 140 parts of 1,1'-oxybisethane are added carefully 106.4 parts of 1H-imidazole. Upon completion, there are added 180 parts of N,N-dimethylformamide and the whole is stirred for 2 hours at 50° C. After the addition of water, the product is extracted twice with trichloromethane. The combined extracts are washed three times with water, dried, filtered and evaporated. The residue is converted into the hydrochloride salt in 4-methyl-2-pentanone, 2,2'-oxybispropane and 2-propanol. The salt is filtered off and crystallized from a mixture of ethanol and 2,2'-oxybispropane, yielding 1.5 parts of 1-(2-chloro-4-fluorophenyl)-2-(1H-imidazol-1-yl)ethanone hydrochloride; mp. 197.4° C.

후처리

  1. extractionthe product is extracted twice with trichloromethane
  2. washThe combined extracts are washed three times with water
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. filtrationThe salt is filtered off
  7. customcrystallized from a mixture of ethanol and 2,2'-oxybispropane

출처 및 근거

ORD 기록
ord-ec6640a85335449abe86bcec9ec70637
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04209447

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