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
A mixture of 10.0 g. (0.033 mole) of 2-(1-piperazinyl)-4-amino-6,7-dimethoxyquinazoline, prepared as described in U.S. Pat. No. 3,511,836, 3.54 g. (0.033 mole) of cyanogen bromide and 33 ml. of N,N-dimethylformamide was stirred under nitrogen at room temperature (20°-25° C.) for 6 hours. The precipitated solid was recovered by filtration, washed with ether and air dried to afford 11.6 g. (85%) of the hydrobromide salt of the title compound. The salt was partitioned between 250 ml. of aqueous saturated sodium bicarbonate solution and 500 ml. of chloroform. The layers were separated and the chloroform layer concentrated in vacuo to afford the free base as a dry foam, 8.3 g. (80%); M.P. 215° C. The mass spectrum reveals a molecular ion peak at M/e 314. Infrared spectrum (CHCl3): peak at 4.5 μ (CN).
WORKUP
后处理
- additionA mixture of 10.0 g
- filtrationThe precipitated solid was recovered by filtration
- washwashed with ether and air
- customdried
- customto afford 11.6 g