HRID568347

反应详情

EQUATION

反应方程式

HRID 568347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8-methyl-6-[4-hydroxyphenyl]-2-(1H)-quinolone (0.30 g) and n-propylisocyanate (0.5 cm3) was heated under reflux in THF (10 cm3) under nitrogen for 50 hours. Methanol (10 cm3) was then added to dissolve solid material, followed by silica (Merck "MK 60.9385" [Trade Mark]) (10 g), and the volatile material was removed in vacuo. The residue was placed on top of a silica column (Merck "MK 60.9385") and eluted with chloroform:methanol, 19:1. Combination and evaporation of appropriate fractions in vacuo gave a solid which was recrystallised from propan-2-ol to afford the title compound, m.p. 224°-228°, (0.28 g).

WORKUP

后处理

  1. dissolutionto dissolve solid material
  2. customthe volatile material was removed in vacuo
  3. washeluted with chloroform
  4. customCombination and evaporation of appropriate fractions in vacuo
  5. customgave a solid which
  6. customwas recrystallised from propan-2-ol