HRID2373644
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
- 100 °C
PROCEDURE
实验过程
A mixture of 2-methyl-5-(1-piperazinyl)quinazoline (50 mg), 2-{3-[(methylsulfonyl)amino]phenyl}ethyl methanesulfonate (65 mg), diisopropylethylamine (192 μL) and DMF (0.5 mL) was heated to 100° C. in a sealed tube and stirred for 24 hours. The mixture was cooled to room temperature and partitioned between aqueous ammonium chloride solution and ethyl acetate. The organic layer was washed (water, brine), dried (sodium sulfate) and concentrated in vacuo. The residue was purified by column chromatography [SiO2; DCM-MeOH: (100:0)→(95:5)] to give the title compound as a beige foam (35 mg).
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- custompartitioned between aqueous ammonium chloride solution and ethyl acetate
- washThe organic layer was washed (water, brine)
- dry with materialdried (sodium sulfate)
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography [SiO2; DCM-MeOH: (100:0)→(95:5)]