HRID606333

反应详情

EQUATION

反应方程式

HRID 606333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated
  2. temperatureto reflux for 3 h
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customThe crude product was purified by column chromatography (silica gel, 5→10% EtOAc in Hexane)
  5. customrecrystallized from EtOAc/Hexane