HRID1726987
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a cooled suspension (−10° C.) of 0.9 g (3.38 mmol) of 4-benzyloxy-5,6,7,8-tetrahydronaphthalene-1-carboxaldehyde [PCT Int. Appl. (2002), WO2002/092084A1] in 10 ml of absolute ethanol were added successively 0.75 ml (3.7 mmol) of triethyl phosphonoacetate and 0.255 g (3.7 mmol) of powdered sodium ethylate. Then, the mixture was stirred at ambient temperature for 1 hour. Subsequently, the reaction mixture was poured onto crushed ice/diluted hydrochloric acid and the product was extracted twice with tert.-butyl methyl ether; the organic phase was washed with brine and dried over anhydrous sodium sulfate, and finally evaporated leaving 1.15 g of the title compound as light brown solid.
WORKUP
后处理
- additionSubsequently, the reaction mixture was poured
- customonto crushed ice/diluted hydrochloric acid
- extractionthe product was extracted twice with tert.-butyl methyl ether
- washthe organic phase was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customfinally evaporated