Urea → N-(Carbamoylcarbamothioyl)-4-chlorobenzamide
反応式
[Cl:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([N:8]=[C:9]=[S:10])=[O:7])=[CH:4][CH:3]=1.[NH2:13][C:14]([NH2:16])=[O:15]>CC(C)=O>[C:14]([NH:16][C:9]([NH:8][C:6](=[O:7])[C:5]1[CH:11]=[CH:12][C:2]([Cl:1])=[CH:3][CH:4]=1)=[S:10])(=[O:15])[NH2:13]参加物
4
実験手順
4-Chlorobenzoyl isothiocyanate (395 mg) and 600 mg urea (5 equiv) were mixed in 30 mL of acetone and stirred at reflux for 1 day. The reaction was concentrated and the residue slurried in diethyl ether. The residue was collected by filtration and washed with diethyl ether. The white solid was dissolved in ethyl acetate (10 ml) and the resultant solution washed with water (10 ml) and brine (10 ml), dried over MgSO4, filtered and concentrated to a white solid (0.35 g, 1.4 mmol, 70% yield.
後処理
- temperatureat reflux for 1 day
- concentrationThe reaction was concentrated
- filtrationThe residue was collected by filtration
- washwashed with diethyl ether
- dissolutionThe white solid was dissolved in ethyl acetate (10 ml)
- washthe resultant solution washed with water (10 ml) and brine (10 ml)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated to a white solid (0.35 g, 1.4 mmol, 70% yield
出典と根拠
- ORDレコード
- ord-fe371120aa564ab7b91f45e7ba280c97
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09162994B2
反応ノート
読み込み中…