HRID507745
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
- 60 °C
PROCEDURE
实验过程
Compound 28 (0.65 g, 0.62 mmol) was dissolved in dimethylacetamide and 0.4 g of compound 14 (1.2 mmol) was added to the reaction mixture as a solid. The reaction mixture was heated to 60° C. for 6 hours, then let cool to room temperature and 80 ml diethyl ether added and let stand for 3 days. The supernatant was decanted off leaving a dark brown residue, which was purified by flash silica chromatography (5 to 10% MeOH/CH2Cl2 then 5 to 10% MeOH/CH2Cl2 W/1% NH4OH) to give 0.45 g (0.37 mmol, 60%) of a yellow solid (compound 30).
WORKUP
后处理
- temperaturelet cool to room temperature
- customThe supernatant was decanted off
- customleaving a dark brown residue, which
- customwas purified by flash silica chromatography (5 to 10% MeOH/CH2Cl2