Sodium Acetate → 2-[[3-Methyl-1-(4-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid

HRID 497997

반응식

HRID 497997 반응식
O=[C:2]([CH3:15])[CH2:3][C:4]1[O:9][C:8](=[O:10])[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[N:5]=1.Cl.[NH:17]([C:19]1[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=1)[NH2:18].C([O-])(=O)C.[Na+]>C(O)C>[CH3:15][C:2]1[CH:3]=[C:4]([NH:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8]([OH:9])=[O:10])[N:17]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)[N:18]=1

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 159380972-(2-Oxo-propyl)-benzo[D][1,3]oxazin-4-oneHCID 223202584-Hydrazinylpyridine hydrochloride

생성물 1

HCID 223202272-[[3-Methyl-1-(4-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid수율 49.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2-(2-oxopropyl)-4H-3,1-benzoxazin-4-one (16.7 g, 82.4 mmol), 4-hydrazinopyridine hydrochloride (12.0 g, 82.4 mmol) and sodium acetate (8.10 g, 98.9 mmol) in ethanol (300 mL) was heated under reflux for 30 minutes. The solution was cooled to room temperature and concentrated under reduced pressure. The residue was poured into water and the resulting crude crystals were collected by filtration. The crystals were washed with ethanol and air dried to give the title compound (11.9 g, 49% yield).

후처리

  1. temperatureunder reflux for 30 minutes
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue was poured into water
  4. filtrationthe resulting crude crystals were collected by filtration
  5. washThe crystals were washed with ethanol and air
  6. customdried

출처 및 근거

ORD 기록
ord-59f508b342ef4dfb8bbe3d56c92b80dc
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949648B2

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