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
- 120 °C
PROCEDURE
实验过程
A glass microwave reaction vessel was charged with N1,N1-bis(2-methoxyethyl)-3-methylbutane-1,3-diamine (50 mg, 0.229 mmol) and 8-iodo-3-methyl-2-(methylsulfinyl)quinazolin-4(3H)-one (700b; 80 mg, 0.229 mmol) in tBuOH (0.5 mL). The reaction mixture was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc.) at 120° C. for 45 min. Similarly another two batches (50 mg and 170 mg) were carried out. The three batches were combined and the solvent was removed. The residue was purified with silica gel chromatography (eluted with 0-5% MeOH in DCM) to give 2((4-(bis(2-methoxyethyl)amino)-2-methylbutan-2-yl)amino)-8-iodo-3-methylquinazolin-4(3H)-one (210 mg, 0.42 mmol). MS (ESI, pos. ion) m/z: 503 (M+1).
WORKUP
后处理
- customA glass microwave reaction vessel
- customthe solvent was removed
- customThe residue was purified with silica gel chromatography (eluted with 0-5% MeOH in DCM)