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Tetrahydrofuran → 2-(2,4-Difluorophenyl)-1-(3-ethoxyphenyl)-1H-imidazole-4-carboxylic acid

HRID 2356596
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HRID 2356596 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=2[F:20])=[NH:12])[CH:7]=[CH:8][CH:9]=1)[CH3:2].C[Si]([N-][Si](C)(C)C)(C)C.[Na+].C([O:33][C:34]1C=C(C=[CH:39][CH:40]=1)N)C.FC1C=C(F)C=CC=1C#N.[O:51]1CCCC1>[Cl-].[Na+].O.ClCCl>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([N:10]2[CH:39]=[C:40]([C:34]([OH:33])=[O:51])[N:12]=[C:11]2[C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=2[F:20])[CH:7]=[CH:8][CH:9]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 8028TetrahydrofuranHCID 121203-EthoxyanilineHCID 775452,4-DifluorobenzonitrileHCID 2724254Sodium bis(trimethylsilyl)amideHCID 178466610HCID 178466610, 화합물

생성물 1

HCID 534142232-(2,4-Difluorophenyl)-1-(3-ethoxyphenyl)-1H-imidazole-4-carboxylic acid

시약·촉매·용매

2
HCID 6344Dichloromethane용매HCID 57417360Sodium chloride; water용매

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온도
-78 °C

실험 절차

N-(3-Ethoxyphenyl)-2,4-difluorobenzenecarboximidamide To a solution of 2.2 ml (4.4 mmol) of 2.0 M (in tetrahydrofuran) sodium bis(trimethylsilyl)amide in 10 mL of tetrahydrofuran at ambient temperature was added 0.52 mL (4.0 mmol) of 3-ethoxyaniline and the resulting solution was stirred for 20 min. The reaction mixture was cooled to −78° C. and then was added 0.57 ml (4.0 mmol) of 2,4-difluorobenzonitrile. The resulting mixture was stirred from −78° C. to ambient temperature for 5 hrs and then poured into brine (25 mL) and dichloromethane (50 mL). The organic layer was separated and the aqueous layer was extracted with dichloromethane (25 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. Flash chromatography on a Biotage Horizon® system (silica gel, 0 to 50% ethyl acetate in hexanes gradient) gave the title compound as a yellow oil. LC/MS 277.2 (M+1).

후처리

  1. stirringThe resulting mixture was stirred from −78° C. to ambient temperature for 5 hrs
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with dichloromethane (25 mL)
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-388353a10fa74a2a877748f71b739f27
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759352B2

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