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
Sodium hydride (0.057 g, 1.4 mmol, 60% mineral oil dispersion) is suspended in anhydrous THF (5 mL) and treated with a solution of (2-oxopyrrolidin-3-(S)-yl)-carbamic acid tert-butyl ester (0.223 g, 1.1 mmol) and 7-bromomethyl-1-chloro-6-methoxy-isoquinoline (0.32 g, 1.1 mmol) in THF/DMF (10 mL, 6:1) at 0° C. The reaction mixture is warmed to ambient temperature, stirred for 3 hours, quenched by the addition of saturated NH4Cl and diluted with EtOAc. The layers are separated. The organic layer is washed with saturated NaCl, dried over Na2SO4, filtered, and concentrated to give a white solid. The solid is collected, washed with a small amount of EtOAc and copious amounts of Et2O to yield the title compound (0.18 g, 0.47 mmol).
WORKUP
后处理
- customquenched by the addition of saturated NH4Cl
- additiondiluted with EtOAc
- customThe layers are separated
- washThe organic layer is washed with saturated NaCl
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customto give a white solid
- customThe solid is collected
- washwashed with a small amount of EtOAc and copious amounts of Et2O