HRID1713975
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 1-(3-aminopropyl)-2-pyrrolidinone (560 μL, 4 mmol) and benzoyl isothiocyanate (536 μL, 4 mmol) was dissolved in chloroform (3 mL), stirred at room temperature for 30 min, then concentrated in vacuo. The resulting residue was dissolved in concentrated HCl (3 mL), heated at 95° C. for 2 h, then concentrated in vacuo. The resulting residue was dissolved in water and washed with dichloromethane (2×30 mL), then basified with 2 M NaOH and extracted with dichloromethane (2×30 mL). The combined extracts were dried over MgSO4 and concentrated to provide 1-(3-(2-oxopyrrolidin-1-yl)propyl)thiourea (638 mg) as a pale yellow oil.
WORKUP
后处理
- concentrationconcentrated in vacuo
- dissolutionThe resulting residue was dissolved in concentrated HCl (3 mL)
- temperatureheated at 95° C. for 2 h
- concentrationconcentrated in vacuo
- dissolutionThe resulting residue was dissolved in water
- washwashed with dichloromethane (2×30 mL)
- extractionextracted with dichloromethane (2×30 mL)
- dry with materialThe combined extracts were dried over MgSO4
- concentrationconcentrated