Hydrazinecarboxaldehyde → Formic acid [1-(3-chloro-4-pyridinyl)ethylidene]hydrazide
反応式
[C:1]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[Cl:10])(=O)[CH3:2].[CH:11]([NH:13][NH2:14])=[O:12]>C(O)C>[Cl:10][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][C:4]=1[C:1](=[N:14][NH:13][CH:11]=[O:12])[CH3:2]参加物
4
実験手順
A mixture of 6.30 gm (0.0405 mole) of 4-acetyl-3-chloropyridine, 2.46 gm (0.041 mole) of formic acid hydrazide and 100 ml of ethanol was refluxed 18 hr. The mixture was chilled in the freezer to give a solid which was collected in two crops. The product was purified by chromatography [keiselgel 60 (230-400 mesh)] and eluting with 5% methanol/methylene chloride to give 2.56 gm (32%) of white flakes which have a melting point of 175.2° C.
後処理
- temperaturewas refluxed 18 hr
- temperatureThe mixture was chilled in the freezer
- customto give a solid which
- customwas collected in two crops
- customThe product was purified by chromatography [keiselgel 60 (230-400 mesh)]
- washeluting with 5% methanol/methylene chloride
- customto give 2.56 gm (32%) of white flakes which
出典と根拠
- ORDレコード
- ord-017b4feb19a1469688de91e821d30bb7
- 出典データセット
- uspto-grants-1991_04
- 特許番号
- US05011932
反応ノート
読み込み中…