HRID1384169
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
Potassium tert-butoxide (3 g, 26.5 mmol) is added to a solution of methyl 3-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-2-naphthylcarbonyl)benzoate (6.6 g, 18.9 mmol) and methyltriphenylphosphonium bromide (9.4 g, 26.3 mmol) in THP (60 ml). The mixture is stirred for 1 h at room temperature. The solution is extracted with ethyl acetate. After separation of the phases by settling, the organic phase is washed twice with 40 ml of water, dried over anhydrous magnesium sulphate and concentrated on a rotary evaporator under vacuum at 40° C. The product is purified by flash chromatography on a column of silica.
WORKUP
后处理
- extractionThe solution is extracted with ethyl acetate
- customAfter separation of the phases
- washthe organic phase is washed twice with 40 ml of water
- dry with materialdried over anhydrous magnesium sulphate
- concentrationconcentrated on a rotary evaporator under vacuum at 40° C
- customThe product is purified by flash chromatography on a column of silica