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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A suspension of 1-{3-[(2-{[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]oxy]ethyl)oxy}phenyl}methanamine obtained in Reference Example 32 (300 mg, 1.18 mmol) and ethyl 5,6-difluoro-4-oxo-3,4-dihydroquinazoline-2-carboxylate obtained in Reference Example 57 (562 mg, 1.18 mmol) in ethanol (10 mL) was stirred at 80° C. for 12 hr. The insoluble material was filtered off hot, and the filtrate was allowed to cool to room temperature. The precipitated solid was collected by filtration using glass filter, and the obtained solid was washed with diethyl ether to give 5,6-difluoro-4-oxo-N-({3-[(2-{[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]oxy}ethyl)oxy]phenyl}methyl)-3,4-dihydroquinazoline-2-carboxamide as a pale-yellow powder (330 mg, 41%).
WORKUP
后处理
- filtrationThe insoluble material was filtered off hot
- temperatureto cool to room temperature
- filtrationThe precipitated solid was collected by filtration
- filtrationfilter
- washthe obtained solid was washed with diethyl ether