HRID63927
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
- 0 °C
PROCEDURE
实验过程
To a mixture of 5-(4-chlorobenzyl)-6-(3-chlorophenyl)furo[2,3-d]pyrimidine-2,4(1H,3H)-dione (38.7 mg, 0.1 mmol) and K2CO3 (13.8 mg, 0.1 mmol) in DMF (1 mL) at 0° C. was added chloromethyl-2-trimethylsilylethyl ether (33.4 mg, 0.2 mmol). The reaction was stirred at 0° C. for 1 h then diluted with EA (10 mL) and water (3 mL). The organic layer was washed with brine (3 mL), dried over Na2SO4 and concentrated to a residue which was purified by chromatography eluted with PE/EA (5:1) to give 5-(4-chlorobenzyl)-6-(3-chlorophenyl)-1-((2-(trimethylsilyl)ethoxy)methyl)furo[2,3-d]pyrimidine-2,4(1H,3H)-dione (31 mg, 60.7% yield) as a colorless oil. LCMS: MH+ 517 and TR=2.196 min.
WORKUP
后处理
- washThe organic layer was washed with brine (3 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated to a residue which
- customwas purified by chromatography
- washeluted with PE/EA (5:1)