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Imidazole → HCID 59333320, 화합물

HRID 1893441
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HRID 1893441 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.I[C:7]1[CH:12]=[CH:11][C:10]([O:13][C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=1[N+:18]([O-:20])=[O:19]>C(OCC)(=O)C>[N+:18]([C:8]1[CH:9]=[C:10]([O:13][C:14]([F:15])([F:16])[F:17])[CH:11]=[CH:12][C:7]=1[N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)([O-:20])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 795ImidazoleHCID 27826691-Iodo-2-nitro-4-(trifluoromethoxy)benzene2회

생성물 1

HCID 59333320HCID 59333320, 화합물수율 69.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

1H-imidazole (818 mg, 12 mmol, 4 eq) and 1-iodo-2-nitro-4-(trifloromethoxy)benzene (1.0 g, 3 mmol, 1 eq) under argon are heated with a heat-gun at between 300 and 500° C. for 45 min until 1-iodo-2-nitro-4-(trifluoromethoxy)benzene has completely reacted on TLC monitoring. The crude mixture is cooled to room temperature, diluted in ethyl acetate and washed with a saturated solution of ammonium chloride. The organic phase is dried over sodium sulfate and concentrated under vacuum. Purification on silica gel (95/05 dichloromethane/methanol) afforded the title compound (570 mg, 2.08 mmol, 69%) as a yellow powder.

후처리

  1. customhas completely reacted on TLC monitoring
  2. washwashed with a saturated solution of ammonium chloride
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. concentrationconcentrated under vacuum
  5. customPurification on silica gel (95/05 dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-167bd396c2b345b6a74da459aba737ea
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08513250B2

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