Hydrochloric Acid → 2-Pyridin-2-yl-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 889306ノート

反応式

HRID 889306 の反応式
C([O:3][C:4](=O)[CH:5]([C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[CH:6]=[N:7][NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)C.C([O-])C.[Na+].Cl>C(O)C>[N:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[N:8]1[C:4](=[O:3])[C:5]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[CH:6][NH:7]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 687052862-Pyridin-3-yl-3-(pyridin-2-ylhydrazono)propionic acid ethyl ester

生成物 1

HCID 591869472-Pyridin-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

3.95 g (13.9 mmol) of the compound from Example 3A are initially introduced into 80 ml ethanol under argon and 945 mg (13.9 mmol) sodium ethanolate are added in portions at RT. After stirring for 30 min, 13.9 ml 1 M hydrochloric acid are added dropwise. The precipitate which has separated out is filtered off with suction, washed with cold ethanol (20 ml) and with water (twice with 20 ml each time) and dried in vacuo. 2.80 g (85% of th.) of the title compound are obtained.

後処理

  1. customThe precipitate which has separated out
  2. filtrationis filtered off with suction
  3. washwashed with cold ethanol (20 ml) and with water (twice with 20 ml each time) and
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-ef843123af2949c3a892d2f4d595be26
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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