HRID1929411
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
- 120 °C
PROCEDURE
实验过程
Ethyl 4-iodobenzoate (276 mg), (1R,2R,3R,5S)-2,6,6-trimethylbicyclo[3.1.1]heptan-3-ol (154 mg), 1,10-phenanthroline (36 mg), copper iodide (19 mg) and cesium carbonate (652 mg) were combined in toluene (0.5 mL). The reaction was heated to 120° C. over 36 hours. The reaction mixture was removed from heat, allowed to cool, diluted with ethyl acetate and poured into water. The organic layer was washed thoroughly with water and brine, dried over MgSO4, filtered and concentrated under vacuum. The crude material was purified by flash chromatography eluting with 95/5 hexanes/ether.
WORKUP
后处理
- customThe reaction mixture was removed
- temperaturefrom heat
- temperatureto cool
- additiondiluted with ethyl acetate
- additionpoured into water
- washThe organic layer was washed thoroughly with water and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under vacuum
- customThe crude material was purified by flash chromatography
- washeluting with 95/5 hexanes/ether