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
To a suspension of 7-(5-fluoro-2-methylphenyl)isoquinolin-3-amine (0.5145 g, 2.039 mmol) in 1,2-dichloroethane (10 mL, 100 mmol) was added triethylamine (0.35 mL, 2.5 mmol) and p-nitrophenyl chloroformate (0.452 g, 2.24 mmol). The reaction mixture was stirred at room temperature for 16 hours and then pyridine (0.50 mL, 6.2 mmol) and p-nitrophenyl chloroformate (0.452 g, 2.24 mmol) were added. After an additional 2 hours, the reaction mixture was diluted with dichloromethane, washed with saturated aqueous NaHCO3, dried over MgSO4, and evaporated in vacuo. 1.069 g of 4-nitrophenyl 7-(5-fluoro-2-methylphenyl)isoquinolin-3-ylcarbamate was obtained, and carried forward without purification. LCMS (ESI): M+H=poor ionization.
WORKUP
后处理
- waitAfter an additional 2 hours
- washwashed with saturated aqueous NaHCO3
- dry with materialdried over MgSO4
- customevaporated in vacuo