Ethanol → 1-(4-Cyanophenyl)-4-hydroxycarbonyl-2-methyl-3-[4-(2-pyridyl)phenyl]-2H-pyrazol-5-one

HRID 1740085ノート

反応式

HRID 1740085 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13](=[O:14])[C:12]([C:15]([O:17]CC)=[O:16])=[C:11]([C:20]3[CH:25]=[CH:24][C:23]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=4)=[CH:22][CH:21]=3)[N:10]2[CH3:32])=[CH:5][CH:4]=1)#[N:2].C(=O)([O-])[O-].[K+].[K+].C(O)C>O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([N:9]2[C:13](=[O:14])[C:12]([C:15]([OH:17])=[O:16])=[C:11]([C:20]3[CH:25]=[CH:24][C:23]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=4)=[CH:22][CH:21]=3)[N:10]2[CH3:32])=[CH:7][CH:8]=1)#[N:2]

参加物

5

反応物 3

HCID 702EthanolHCID 11430Potassium CarbonateHCID 218376381-(4-cyanophenyl)-4-ethoxycarbonyl-2-methyl-3-[4-(2-pyridyl)phenyl]-2H-pyrazol-5-one

生成物 1

HCID 218376341-(4-Cyanophenyl)-4-hydroxycarbonyl-2-methyl-3-[4-(2-pyridyl)phenyl]-2H-pyrazol-5-one収率 63.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2.7 g of 1-(4-cyanophenyl)-4-ethoxycarbonyl-2-methyl-3-[4-(2-pyridyl)phenyl]-2H-pyrazol-5-one, 1.8 g of potassium carbonate, 73 ml of ethanol and 8 ml of water was refluxed under heating for 9 hours. The reaction solution was cooled to room temperature, and the precipitated crystals were collected by filtration and dried under reduced pressure. The resulting crude crystals were suspended in chloroform, and the suspension was adjusted to pH 2 to 3 with dilute hydrochloric acid. The crystals were collected by filtration and dried under reduced pressure to give 1.6 g of the title compound as pale gray crystals.

後処理

  1. temperaturewas refluxed
  2. temperatureunder heating for 9 hours
  3. filtrationthe precipitated crystals were collected by filtration
  4. customdried under reduced pressure
  5. filtrationThe crystals were collected by filtration
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-d4ba679ec8e644109add6a8d10145440
出典データセット
uspto-grants-1999_10
特許番号
US05968967

反応ノート

読み込み中…