Thioacetamide → 3,4-Diethoxybenzamide
反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[O:12][CH2:13][CH3:14])[C:7]#[N:8])[CH3:2].C(N)(=S)C.Cl.CN(C)C=[O:23]>>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[O:12][CH2:13][CH3:14])[C:7]([NH2:8])=[O:23])[CH3:2]参加物
4
反応条件
- 温度
- 130 °C
実験手順
In 120 ml of 10% hydrochloric acid-dimethylformamide were dissolved 29 g of 3,4-diethoxybenzonitrile and 23 g of thioacetamide. The solution was heated at 90° C. for 3 hours and further at 130° C. for 5 hours to conduct a reaction. The reaction mixture was subjected to distillation to remove the solvent. The residue was washed twice with 100 ml of diethyl ether, followed by washing with 100 ml of water. The resulting crystals were collected by filtration and dried to obtain 21.7 g of 3,4-diethoxybenzamide.
後処理
- customa reaction
- distillationThe reaction mixture was subjected to distillation
- customto remove the solvent
- washThe residue was washed twice with 100 ml of diethyl ether
- washby washing with 100 ml of water
- filtrationThe resulting crystals were collected by filtration
- customdried
出典と根拠
- ORDレコード
- ord-2e74b48555d0458f88c4a448e6027f25
- 出典データセット
- uspto-grants-1997_06
- 特許番号
- US05639770
反応ノート
読み込み中…