HRID21406
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
Thionyl chloride (0.5 ml) was added, dropwise, to a! stirred solution of 4-hydroxy-3-methoxyphenethyl alcohol (0.83 g--commercially available) in dichloromethane (50 ml). When the addition was complete, the mixture was heated under reflux for 3 hours. On cooling to room temperature, the mixture was concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 2%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as an oil, yield 0.36 g.
WORKUP
后处理
- additionWhen the addition
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hours
- concentrationthe mixture was concentrated in vacuo
- customto give a gum which
- customwas purified by column chromatography on silica eluting with dichloromethane
- additioncontaining methanol (0% up to 2%)
- concentrationconcentrated in vacuo