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Hydrochloric Acid → 2-(4-Methylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 889303
ノート
印刷プレビュー

反応式

HRID 889303 の反応式
C(O[C:4](=[O:14])[C:5]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=[CH:6]O)C.[NH:15]([C:17]1[CH:22]=[C:21]([CH3:23])[CH:20]=[CH:19][N:18]=1)[NH2:16].C([O-])C.[Na+].Cl>C(O)C>[CH3:23][C:21]1[CH:20]=[CH:19][N:18]=[C:17]([N:15]2[C:4](=[O:14])[C:5]([C:8]3[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=3)=[CH:6][NH:16]2)[CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 122667392-Hydrazinyl-4-methylpyridineHCID 687080883-Hydroxy-2-pyridin-3-yl-acrylic acid ethyl ester

生成物 1

HCID 591869542-(4-Methylpyridin-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

1.53 g (7.90 mmol) of the compound from Example 2A and 2.92 g (23.7 mmol) of the compound from Example 1A are dissolved 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 16 h. 537 g (7.90 mmol) sodium ethanolate are added, the reaction solution becoming dark red in color. The mixture is subsequently stirred at RT for 30 min and 7.9 ml 1 M hydrochloric acid are then added. The solution is partly concentrated, a precipitate separating out. This is filtered off, washed with water (twice with 5 ml each time) and with MTBE (5 ml) and dried in vacuo. 435 mg (22% of th.) of the title compound are obtained.

後処理

  1. stirringThe mixture is subsequently stirred at RT for 30 min
  2. concentrationThe solution is partly concentrated
  3. customa precipitate separating out
  4. filtrationThis is filtered off
  5. washwashed with water (twice with 5 ml each time) and with MTBE (5 ml)
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-63bf55f4b9034805bcbdb450d41003c6
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252817B2

反応ノート

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