HRID1527702
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
PROCEDURE
实验过程
Following a modified procedure of Smith et al.,25 dibromide 36 (1.73 g, 4.80 mmol) was dissolved in 1,2-dimethoxyethane (50.0 mL), and then added to CaCO3 (2.50 g, 25.0 mmol) in H2O (50.0 mL) at room temperature. The reaction was heated under reflux for TIME and then cooled to room temperature. The reaction was extracted with EtOAc (75.0 mL), and the organic layers are washed with brine. The organic layer was dried over MgSO4 and filtered. The resulting pink solid was then purified by flash column chromatography (1:3 EtOAc:hexanes) to provide 37 (1.49 g, 5.01 mmol, 105%) as a pink solid.
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureunder reflux for TIME
- extractionThe reaction was extracted with EtOAc (75.0 mL)
- washthe organic layers are washed with brine
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- customThe resulting pink solid was then purified by flash column chromatography (1:3 EtOAc:hexanes)