Urea → N-(Carbamoylcarbamothioyl)-4-chlorobenzamide
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-fe371120aa564ab7b91f45e7ba280c97
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09162994B2
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