p-Toluenesulfonic acid → 2-(4,5-Dimethylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 1913204ノート

反応式

HRID 1913204 の反応式
CN(C)[CH:3]=[C:4]([C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)[C:5](OCC)=[O:6].[NH:17]([C:19]1[CH:24]=[C:23]([CH3:25])[C:22]([CH3:26])=[CH:21][N:20]=1)[NH2:18].C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)C>[CH3:25][C:23]1[C:22]([CH3:26])=[CH:21][N:20]=[C:19]([N:17]2[C:5](=[O:6])[C:4]([C:10]3[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=3)=[CH:3][NH:18]2)[CH:24]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 552791581154030-52-0HCID 687048643-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester

生成物 1

HCID 592801902-(4,5-Dimethylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

220 mg (1.0 mmol) of the compound from Example 2A are initially charged in 5 ml of ethanol. 137 mg (1.0 mmol) of the compound from Example 21A and 38 mg (0.2 mmol) of p-toluenesulfonic acid are added, and the mixture is stirred under reflux for 16 h. The mixture is then allowed to cool to RT, and the solid formed is filtered off, washed with tert-butyl methyl ether and dried under high vacuum. This gives 28 mg of the title compound. The mother liquor is put aside and used for preparing the hydrochloride (see Example 87).

後処理

  1. temperatureunder reflux for 16 h
  2. customthe solid formed
  3. filtrationis filtered off
  4. washwashed with tert-butyl methyl ether
  5. customdried under high vacuum
  6. customused for preparing the hydrochloride (see Example 87)

出典と根拠

ORDレコード
ord-160c512f588e4d75a9c22877d81ae7f1
出典データセット
uspto-grants-2013_12
特許番号
US08609698B2

反応ノート

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