HCID 178505869, 화합물 → HCID 178507659, 화합물

HRID 45844노트

반응식

HRID 45844 반응식
C([N:8](CC1C=CC=CC=1)[C:9]1[CH:14]=[CH:13][C:12]([F:15])=[C:11]([C:16]2[C:20]([C:21]3[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=3)=[CH:19][NH:18][N:17]=2)[C:10]=1[F:27])C1C=CC=CC=1>CO.[OH-].[OH-].[Pd+2]>[F:27][C:10]1[C:11]([C:16]2[C:20]([C:21]3[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=3)=[CH:19][NH:18][N:17]=2)=[C:12]([F:15])[CH:13]=[CH:14][C:9]=1[NH2:8]

참가 물질

4

반응물 1

HCID 178505869HCID 178505869, 화합물

생성물 1

HCID 178507659HCID 178507659, 화합물수율 56%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매

실험 절차

To dibenzyl-[2,4-difluoro-3-(4-pyridin-4-yl-1H-pyrazol-3-yl)-phenyl]-amine (1.795 g, 3.97 mmol) in methanol (100 mL) was added 20% palladium hydroxide on carbon (646 mg). The reaction was stirred under hydrogen atmosphere for 12 hours (45 psi). The reaction was filtered to remove the catalyst, and then concentrated under reduced pressure. The crude was purified by silica gel column chromatography eluting with methanol 7% in methylene chloride to give 2,4-difluoro-3-(4-pyridin-4-yl-1H-pyrazol-3-yl)-phenylamine (yield 56% over three steps).

후처리

  1. filtrationThe reaction was filtered
  2. customto remove the catalyst
  3. concentrationconcentrated under reduced pressure
  4. customThe crude was purified by silica gel column chromatography
  5. washeluting with methanol 7% in methylene chloride

출처 및 근거

ORD 기록
ord-a9ae1a1bae8e4319b2e90a64f21b9ba1
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541575B2

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