Hydrochloric Acid → 2-Pyridin-2-yl-4-(6-trifluormethylpyridin-3-yl)-1,2-dihydro-3h-pyrazol-3-one

HRID 889309ノート

反応式

HRID 889309 の反応式
C(O[C:4](=[O:18])[C:5]([C:8]1[CH:9]=[N:10][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:12][CH:13]=1)=[CH:6]O)C.[NH:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1)[NH2:20].C([O-])C.[Na+].Cl>C(O)C>[N:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[N:19]1[C:4](=[O:18])[C:5]([C:8]2[CH:9]=[N:10][C:11]([C:14]([F:15])([F:16])[F:17])=[CH:12][CH:13]=2)=[CH:6][NH:20]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 786452-HydrazinopyridineHCID 2723922Sodium ethoxideHCID 687048893-Hydroxy-2-(6-trifluoromethylpyridin-3-yl)-acrylic acid ethyl ester

生成物 1

HCID 591869752-Pyridin-2-yl-4-(6-trifluormethylpyridin-3-yl)-1,2-dihydro-3h-pyrazol-3-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

261 mg (1.00 mmol) of the compound from Example 41A and 115 mg (1.05 mmol) 2-hydrazinopyridine are dissolved in 5 ml anhydrous ethanol under argon and the mixture is stirred at RT for 20 h. 68 mg (1.00 mmol) sodium ethanolate are added, the mixture is stirred at RT for 30 min and 1 M hydrochloric acid and a little ethanol are then added, a precipitate separating out. This is filtered off, washed with a little ethanol and dried in vacuo.

後処理

  1. stirringthe mixture is stirred at RT for 30 min
  2. customa precipitate separating out
  3. filtrationThis is filtered off
  4. washwashed with a little ethanol
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-15a70f4d75eb4fd08071d8521301a8c6
出典データセット
uspto-grants-2012_08
特許番号
US08252817B2

反応ノート

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