Hydrochloric Acid → 3-Methyl-1-(3-pyridinyl)-1H-pyrazol-5-ylamine dihydrochloride

HRID 498057

반응식

HRID 498057 반응식
N/[C:2](=[CH:5]\[CH3:6])/[C:3]#[N:4].[ClH:7].Cl.[NH:9]([C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1)[NH2:10].Cl>O>[ClH:7].[ClH:7].[CH3:6][C:5]1[CH:2]=[C:3]([NH2:4])[N:9]([C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)[N:10]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 171324893-Hydrazinylpyridine dihydrochlorideHCID 86589747Aminocrotononitrile

생성물 1

HCID 574176993-Methyl-1-(3-pyridinyl)-1H-pyrazol-5-ylamine dihydrochloride수율 96.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of aminocrotononitrile (8.21 g, 100 mmol) and 3-hydrazinopyridine dihydrochloride (20.7 g, 114 mmol) in water (50 mL) was mixed with conc. hydrochloric acid (15 mL), and the mixture was heated under reflux for 30 minutes. The solution was allowed to cool to room temperature, and the reaction solvent was evaporated under reduced pressure, and the resulting crystals were collected by filtration. The crystals obtained were washed with water and air dried to give the title compound (13.6 g, 55% yield).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. customthe reaction solvent was evaporated under reduced pressure
  4. filtrationthe resulting crystals were collected by filtration
  5. customThe crystals obtained
  6. washwere washed with water and air
  7. customdried

출처 및 근거

ORD 기록
ord-477c0bb6523b4f85baa2fe527a4edd3e
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949648B2

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