Acetic Anhydride → N-(4-cyano-2-iodophenyl)acetamide
反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[I:10].[C:11](OC(=O)C)(=[O:13])[CH3:12]>S(=O)(=O)(O)O.O>[C:11]([NH:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[I:10])(=[O:13])[CH3:12]参加物
5
実験手順
A mixture of 8.54 g (0.035 mole) of 4-amino-3-iodobenzonitrile (31), 16 mL (16.32 g, 0.16 mole) of acetic anhydride and five drops of concentrated sulfuric acid was heated at 70° under reflux for 10 minutes (the mixture became thick when the temperature reached 40° and some manual stirring was required). The reaction mixture was poured over 400 mL of cold water and stirred for 5 minutes to give a white solid which was filtered and dried, yielding 9.48 g (95%) of 32 as white powder, mp 176-181°. Infrared (IR) and NMR analysis gave the following results:
後処理
- temperaturewas heated at 70°
- temperatureunder reflux for 10 minutes (the mixture
- customreached 40°
- stirringstirred for 5 minutes
- customto give a white solid which
- filtrationwas filtered
- customdried
出典と根拠
- ORDレコード
- ord-bb6c986914f84ec58c8a84e6a0d5d17a
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06624153B2
反応ノート
読み込み中…