3-Chloro-3-(3-pyridinyl)-2-propenal → 2-Furanyl[7-(3-pyridinyl)pyrazolo[1,5-a]pyrimidin-3-yl]methanone

HRID 1247947

反応式

HRID 1247947 の反応式
Cl[C:2]([C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[CH:3][CH:4]=O.[NH2:12][C:13]1[C:17]([C:18]([C:20]2[O:21][CH:22]=[CH:23][CH:24]=2)=[O:19])=[CH:16][NH:15][N:14]=1>C(O)(=O)C>[O:21]1[CH:22]=[CH:23][CH:24]=[C:20]1[C:18]([C:17]1[CH:16]=[N:15][N:14]2[C:2]([C:6]3[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=3)=[CH:3][CH:4]=[N:12][C:13]=12)=[O:19]

参加物

4

反応物 2

HCID 538697343-Chloro-3-(3-pyridinyl)-2-propenalHCID 178509268HCID 178509268、化合物

生成物 1

HCID 134758992-Furanyl[7-(3-pyridinyl)pyrazolo[1,5-a]pyrimidin-3-yl]methanone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 0.02 mole of 3-chloro-3-(3-pyridinyl)-2-propenal and 0.02 mole of (3-amino-1H-pyrazol-4-yl)-2-furanyl-methanone in 30 ml of glacial acetic acid was refluxed for 5 hours. The solvent was removed in vacuo and the residue partitioned between saturated aqueous sodium bicarbonate and dichloromethane. The dichloromethane layer was dried over sodium sulfate and passed through a short pad of hydrous magnesium silicate. The eluent was concentrated and the residue crystallized from dichloromethane:hexane to give the desired product as crystals, mp 228°-229° C.

後処理

  1. temperaturewas refluxed for 5 hours
  2. customThe solvent was removed in vacuo
  3. customthe residue partitioned between saturated aqueous sodium bicarbonate and dichloromethane
  4. dry with materialThe dichloromethane layer was dried over sodium sulfate
  5. concentrationThe eluent was concentrated
  6. customthe residue crystallized from dichloromethane

出典と根拠

ORDレコード
ord-ab10334a5142416eb34194ec17d02478
出典データセット
uspto-grants-1985_06
特許番号
US04521422

関連ノート

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