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
- 150 °C
PROCEDURE
实验过程
A suspension of 3-(cyclopentylsulfonyl)propyl methanesulfonate (for example, as prepared for Intermediate 25) (0.081 g, 0.3 mmol), 6-butyl-8-(4-piperidinyloxy)quinoline (for example, as prepared for Intermediate 4) (0.102 g, 0.360 mmol), sodium iodide (40 mg, 0.3 mmol) and sodium hydrogen carbonate (200 mg, 2.39 mmol) in dry DMF (2 ml) was heated in a Smith Creator™ microwave oven at 150° C. for 15 min. The reaction mixture was applied to an SCX-2 cartridge (20 g), preconditioned with methanol. The cartridge was washed with methanol (4×25 ml) and then eluted with 10% aqueous 0.88 s.g. ammonia in methanol (4×25 ml). The solvents were removed in vacuo and the resultant residue purified by MDAP to afford the title compound (53 mg): LCMS RT=2.81 min; ES+ve m/z 459 (M+H)+
WORKUP
后处理
- washThe cartridge was washed with methanol (4×25 ml)
- washeluted with 10% aqueous 0.88 s
- customThe solvents were removed in vacuo
- customthe resultant residue purified by MDAP