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
To a stirring solution of 4-[2-(3-Hydroxymethyl-oxetan-3-ylmethoxy)-3,4-dimethoxy-phenyl]-indan-1-one (Compound 104)(100 mg, 0.2604 mmol) in dichloromethane (15 mL), were added triethylamine (0.1 mL, 0.772 mmol) and ethyl isocyanate (55 mg, 0.78 mmol) and the resultant reaction mixture was heated to 50° C. for 16 h. The reaction mixture was quenched with sodium bi carbonate solution and extracted with dichloromethane (3×). The combined dichloromethane layer was washed with brine and dried over anhydrous sodium sulphate and concentrated under reduced pressure. Purification by column chromatography (silica gel, 0-25% ethyl acetate in pet ether) to afforded the title compound as a solid.
WORKUP
后处理
- customthe resultant reaction mixture
- customThe reaction mixture was quenched with sodium bi carbonate solution
- extractionextracted with dichloromethane (3×)
- washThe combined dichloromethane layer was washed with brine
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated under reduced pressure
- customPurification by column chromatography (silica gel, 0-25% ethyl acetate in pet ether)