反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To an ice cold solution of 7-bromo-2,4-dichloro-6-fluoro-quinazoline (0.35 g, 1.178 mmol) in dichloromethane (15 mL), morpholine (0.566 mL, 0.0066 mol) was slowly added and the reaction was continued for 20 minutes. The reaction mixture was diluted with dichloromethane and washed with water. The organic layer was dried over sodium sulphate and evaporated to provide crude solid. The crude material was purified using column chromatography (60-120 silica gel, 30% ethyl acetate in hexane) to provide the title compound (220 mg, 57%). 1H NMR (300 MHz, DMSO-d6): δ 8.16 (d, J=6.6 Hz, 1H), 8.01 (d, J=9.6 Hz, 1H), 3.83-3.86 (m, 4H), 3.76-3.73 (m, 4H); LC-MS (ESI): Calculated mass: 345.0; Observed mass [M+H]+: 347.8 (RT: 1.70 min).
WORKUP
后处理
- washwashed with water
- dry with materialThe organic layer was dried over sodium sulphate
- customevaporated
- customto provide crude solid
- customThe crude material was purified