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
- 50 °C
PROCEDURE
实验过程
A solution of (5R)-5-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-3-[2-(4-hydroxyphenyl)ethyl]-1,3-oxazolidin-2-one (Example 28 v) (37 mg) in dry DMF (0.4 mL) was treated with caesium carbonate (65 mg) and 3-(4bromobutyl)phenyl acetate (0.2 mmol) as a solution in DMF (0.5 mL). Further DMF was added (1 mL) and the reaction mixture stirred at 50° C. for 24 h. The reaction mixture was cooled to room temperature and concentrated in vacuo in a genevac. The residue was suspended in chloroform and filtered to remove inorganic salts. The filtrate was added to the top of a pre-conditioned NH2 propyl cartridge (1 g). The cartridge was washed with chloroform and methanol and the title compound eluted with 2M NH3-MeOH. LCMS RT=3.86 min
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- concentrationconcentrated in vacuo in a genevac
- filtrationfiltered
- customto remove inorganic salts
- additionThe filtrate was added to the top of a pre-conditioned NH2 propyl cartridge (1 g)
- washThe cartridge was washed with chloroform and methanol
- washthe title compound eluted with 2M NH3-MeOH