HRID5210
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
2-Methoxypropene (10 g) was added over 15 min to a stirred solution of 2-bromo-1-[4-hydroxy-3-(hydroxymethyl)phenyl]ethanone (5 g) and toluene-4-sulphonic acid (0.5 g) in CH2Cl2 (100 ml) at 23°. The mixture was stirred for 3h, filtered through a wad of triethylamine-deactivated silica and evaporated to give an oil. Purification by [FCTS] (300 g) [E] afforded the title compound as an oil (4.8 g) with solidified on cooling. A small sample was crystallised from light petroleum (b.p. 60-80°) to give white crystals m.p. 47-48°.
WORKUP
后处理
- filtrationfiltered through a wad of triethylamine-deactivated silica
- customevaporated
- customto give an oil
- customPurification by [FCTS] (300 g) [E]