HRID61616
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a mixture of 2-[(3-phenyl)phenyl]-7-methoxy-4-oxo-3,4-dihydroquinazolin-6-yl acetate (3.6 g, 9.32 mmole) in SOCl2 (40 mL) was added DMF (1 mL) and the reaction was stirred at reflux for 16 h. The mixture was cooled to RT and then the volatiles were removed in vacuo. The crude product was dissolved in CHCl3 (300 mL) and washed with saturated NaHCO3 solution (3×150 mL), water (2×150 mL) and brine (1×150 mL) and dried with Na2SO4. The solution was concentrated in vacuo to yield 4-chloro-2-[(3-phenyl)phenyl]-7-methoxyquinazolin-6-yl acetate (4.0 g, 9.88 mmole). HPLC retention time 11.12 mins. (5-95-13 method).
WORKUP
后处理
- temperatureat reflux for 16 h
- customthe volatiles were removed in vacuo
- dissolutionThe crude product was dissolved in CHCl3 (300 mL)
- washwashed with saturated NaHCO3 solution (3×150 mL), water (2×150 mL) and brine (1×150 mL)
- dry with materialdried with Na2SO4
- concentrationThe solution was concentrated in vacuo