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

HRID 497997ノート

反応式

HRID 497997 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-59f508b342ef4dfb8bbe3d56c92b80dc
出典データセット
uspto-grants-2005_09
特許番号
US06949648B2

反応ノート

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