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Hydrochloric Acid → 4,5-Bis(4-methoxyphenyl)-2-(2-fluorophenylthio)imidazole

HRID 1995198
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HRID 1995198 반응식
[F:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1N.N([O-])=O.[Na+].Cl.[CH3:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[N:23]=[C:24]([SH:35])[NH:25][C:26]=2[C:27]2[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=2)=[CH:18][CH:17]=1.[OH-].[Na+]>CN(C)C=O.[Cu]>[CH3:34][O:33][C:30]1[CH:31]=[CH:32][C:27]([C:26]2[N:25]=[C:24]([S:35][C:3]3[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=3[F:1])[NH:23][C:22]=2[C:19]2[CH:20]=[CH:21][C:16]([O:15][CH3:14])=[CH:17][CH:18]=2)=[CH:28][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 95842-FluoroanilineHCID 14798Sodium HydroxideHCID 23668193Sodium NitriteHCID 178489021HCID 178489021, 화합물

생성물 1

HCID 128323074,5-Bis(4-methoxyphenyl)-2-(2-fluorophenylthio)imidazole수율 33.3%

시약·촉매·용매 2

HCID 23978Copper촉매HCID 6228Dimethylformamide용매

실험 절차

At 0° a diazonium salt solution prepared from 2.5 g of 2-fluoroaniline, 1.58 g of sodium nitrite, and 10 ml of 6 N hydrochloric acid is added dropwise to a solution of 6.25 g of 4,5-bis(4-methoxyphenyl)-2-mercaptoimidazole in a mixture of 240 ml of dimethylformamide, 10 ml of 2 N sodium hydroxide solution, and 1.45 g of powdered copper. The solution develops a reddish brown color under nitrogen evolution. The mixture is further stirred for 3 hours, concentrated under vacuum, and the residue is distributed between water and ethyl acetate. The organic solution is dried over sodium sulfate and concentrated to dryness under vacuum. The residue is subjected to column chromatography on 500 g of silica gel. Elution with acetone/hexane 2:3 yields 2.71 g of 4,5-bis(4-methoxyphenyl)-2-(2-fluorophenylthio)imidazole having a melting point of 195° after recrystallization from hot diisopropyl ether.

후처리

  1. concentrationconcentrated under vacuum
  2. dry with materialThe organic solution is dried over sodium sulfate
  3. concentrationconcentrated to dryness under vacuum
  4. washElution with acetone/hexane 2:3

출처 및 근거

ORD 기록
ord-4bb6814159784cbc9def6b1b18f0da46
출처 데이터셋
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04402960

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