HRID646502
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
- 150 °C
PROCEDURE
实验过程
1-(2,4-Dihydroxy-5-isopropyl-phenyl)-ethanone (1 eq) was dissolved in DMF and potassium carbonate (2.2 eq) then benzyl bromide (2.2 eq) were added. The suspension was heated, with stirring to 150° C., under nitrogen, for 16 hrs. The solution was cooled to room temperature and the mixture was poured into 1MHCl (aq) then extracted in to ethyl acetate. The organic phases were combined and washed again with 1MHCl (aq) then five times with brine solution. The organic phase was dried over MgSO4, filtered and concentrated in vacuo, to give a solid, which was purified by diethyl ether: hexane (1:1) trituration to give 1-(2,4-Bis-benzyloxy-5-isopropyl-phenyl)-ethanone.
WORKUP
后处理
- temperatureThe suspension was heated
- temperatureThe solution was cooled to room temperature
- additionthe mixture was poured into 1MHCl (aq)
- extractionthen extracted in to ethyl acetate
- washwashed again with 1MHCl (aq)
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a solid, which
- customwas purified by diethyl ether: hexane (1:1) trituration