HRID2084322
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
A mixture of 1-(2-hydroxy-4-prop-2-ynyloxy-phenyl)-propan-1-one (19.8 g, 97 mmol) and N,N-diethylaniline (100 mL) was heated to reflux for 3 h. The reaction mixture was concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, 5→10% EtOAc in Hexane) and thereafter recrystallized from EtOAc/Hexane, to give 8.91 g (45%) of 1-(5-hydroxy-2H-chromen-6-yl)-propan-1-one.
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 3 h
- concentrationThe reaction mixture was concentrated under reduced pressure
- customThe crude product was purified by column chromatography (silica gel, 5→10% EtOAc in Hexane)
- customrecrystallized from EtOAc/Hexane