HRID24242
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
- -78 °C
PROCEDURE
实验过程
To a solution of 1-bromo-2-isopropyl-4-methoxy-benzene (Intermediate 143, 2.20 g, 9.60 mmols) in 50 mL CH2Cl2 at −78° C. was added BBr3 (4.81 g, 19.2 mmols; 19.2 mL of a 1M solution in CH2Cl2). After stirring for 3 hours at −78° C. the solution was warmed to 0° C. for 3 hours and then at 25° C. for 1 hour before being quenched with H2O. The mixture was diluted with Et2O and washed with H2O and saturated aqueous NaCl, dried (Na2SO4) and concentrated under reduced pressure. Column chromatography (2.5-10% EtOAc—hexanes) afforded the title compound as a colorless oil.
WORKUP
后处理
- temperaturewas warmed to 0° C. for 3 hours
- customat 25° C. for 1 hour before being quenched with H2O
- additionThe mixture was diluted with Et2O
- washwashed with H2O and saturated aqueous NaCl
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure