Acetic Anhydride → N-(4-methyl-5-nitropyridin-2-yl)acetamide

反応式

[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([NH2:11])[CH:3]=1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>>[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([NH:11][C:12](=[O:14])[CH3:13])[CH:3]=1

参加物

反応物 2

HCID 7918Acetic Anhydride

HCID 2431652-Amino-4-methyl-5-nitropyridine

生成物 1

HCID 13567013N-(4-methyl-5-nitropyridin-2-yl)acetamide収率 87%

反応条件

温度: 90 °C

実験手順

A mixture of 4-methyl-5-nitropyridin-2-amine (5 g, 32 mmol) and acetic anhydride (20 mL) was heated at 90° C. for 4 hours. After cooling the solvent was evaporated under vacuum. The concentrated mass was dissolved in toluene and evaporated under vacuum. The resulting solid was triturated with diethyl ether and filtered to afford N-(4-methyl-5-nitropyridin-2-yl) acetamide (5.5 g, 87%).

後処理

temperatureAfter cooling the solvent
customwas evaporated under vacuum
dissolutionThe concentrated mass was dissolved in toluene
customevaporated under vacuum
customThe resulting solid was triturated with diethyl ether
filtrationfiltered

出典と根拠

ORDレコード: ord-d06bd54f5f924e2ebe9150a2b1d7623e
出典データセット: uspto-grants-2015_03
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08980911B2

反応ノート

読み込み中…

参加物