HRID399339
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
2 g (8.28 mmol) of epoxide 2j in solution in 5 cm3 of anhydrous DMF were heated to reflux for 5 h. The solution was acidified (pH<1) with 3N HCl, extracted with ether and concentrated, and a 3N sodium hydroxide solution was added to the ether phase (while the mixture was kept stirred for 5 to 10 min), the ether phase was removed and the material washed once with ether. The aqueous phase was acidified using a solution with 3N HCl (pH=1) and extracted with ether (4×30 cm3), dried over MgSO4, filtered and evaporated down. 1.24 g of phenol 4g were obtained as a liquid whose macrobore GC purity was higher than 97%. The yield of phenol 4g was 89%.
WORKUP
后处理
- temperatureto reflux for 5 h
- extractionextracted with ether
- concentrationconcentrated
- additiona 3N sodium hydroxide solution was added to the ether phase (while the mixture
- customwas removed
- washthe material washed once with ether
- extractionextracted with ether (4×30 cm3)
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated down