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

HRID 1526089ノート

反応式

HRID 1526089 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-e6e2cc5e18654ff9b82927e2656b93b3
出典データセット
uspto-grants-2015_07
特許番号
US09085572B2

反応ノート

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