HCID 22139808、化合物 → methyl 3-amino-4-chlorothiophene-2-carboxylate
反応式
C([NH:4][C:5]1[C:9]([Cl:10])=[CH:8][S:7][C:6]=1[C:11]([O:13][CH3:14])=[O:12])(=O)C>CO.Cl>[NH2:4][C:5]1[C:9]([Cl:10])=[CH:8][S:7][C:6]=1[C:11]([O:13][CH3:14])=[O:12]参加物
4
反応条件
- 温度
- 60 °C
実験手順
In a mixture of 50 ml of methanol and 50 ml of concentrated hydrochloric acid, 7 g of methyl 3-acetylamino-4-chlorothiophene-2-carboxylate are stirred at 60° C. for 4 hours, under reflux for 5 hours and at room temperature for another 3 days. Any precipitate that has formed is removed by filtration, and about ⅓ of the volume of the solvent is removed by distillation under reduced pressure. Following addition of about 100 ml of water, the mixture is stirred at room temperature for another 15 minutes and the colorless crystals are filtered off and dried in a stream of air. M.p.: 62-64° C.
後処理
- temperatureunder reflux for 5 hours and at room temperature for another 3 days
- customAny precipitate that has formed
- customis removed by filtration
- customabout ⅓ of the volume of the solvent is removed by distillation under reduced pressure
- additionaddition of about 100 ml of water
- stirringthe mixture is stirred at room temperature for another 15 minutes
- filtrationthe colorless crystals are filtered off
- customdried in a stream of air
出典と根拠
- ORDレコード
- ord-d9754836ba144af19fbd90f03888f088
- 出典データセット
- uspto-grants-2006_05
- 特許番号
- US07049333B2
反応ノート
読み込み中…