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 solution of 2-(3-benzyl-7-chloro-4-oxo-3,4-dihydroquinazolin-2-yl)-2-bromo-N,N-dimethylacetamide (1.4 g, 1 eq.) in of N,N-dimethylformamide (10 ml), was added N-Boc-1,3-diaminopropane (2.8 g, 5 eq.). The reaction was stirred at room temperature for 4 h and then heated to 40° C. The mixture was stirred at 40° C. overnight. Water and ethyl acetate were added to the mixture. The organic layer was washed with saturated sodium bicarbonate, saturated sodium chloride, dried over magnesium sulfate, filtered, and concentrated. The crude product was purified by flash chromatography to give tert-butyl 3-{[1-(3-benzyl-7-chloro-4-oxo-3,4-dihydroquinazolin-2-yl)-2-(dimethylamino)-2-oxoethyl]amino}propylcarbamate (1 g) as a pale yellow solid.
WORKUP
后处理
- temperatureheated to 40° C
- stirringThe mixture was stirred at 40° C. overnight
- washThe organic layer was washed with saturated sodium bicarbonate, saturated sodium chloride
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by flash chromatography