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
81 mg of sodium hydride as a 60% suspension in oil (2.03 mmol) are introduced at room temperature into a 25 ml round-bottomed flask, with stirring and under an argon atmosphere, containing 20 ml of THF and 500 mg of 26 (2.03 mmol). The medium is stirred for 1 hour and 1.1 g (2.34 mmol) of 4-butoxybenzyl bromide are then added. The medium is stirred for 16 hours, 20 ml of EtOAc and 20 ml of water are added to the reaction medium and, after separation of the phases by settling, the organic phase is washed with 10 ml of water. The organic phase is dried, filtered and then evaporated to dryness to give 1.3 g of crude product, which product is chromatographed on a silica cartridge (25 g) with a 90/10 heptane/EtOAc mixture. 420 mg of product 39 are recovered (yield=53%).
WORKUP
后处理
- stirringThe medium is stirred for 1 hour
- stirringThe medium is stirred for 16 hours
- customafter separation of the phases
- washthe organic phase is washed with 10 ml of water
- customThe organic phase is dried
- filtrationfiltered
- customevaporated to dryness