HRID255495

反应详情

EQUATION

反应方程式

HRID 255495 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 5-chloro-7-amino-8-hydroxyquinoline (6 g, 30.8 mol) and methyl trimethoxyacetate (16.3 g, 123.2 mol) was heated at 100° C. overnight. The reaction was cooled in an ice bath and filtered. The precipitate was dissolved in acetone (250 ml). The resulting solution was treated with charcoal at reflux, filtered through a pad of silica gel and celite and partially concentrated. Crystals formed which were filtered and dried giving 4.1 g (51% yield) of solid. M.P. 217°-218° C.

WORKUP

后处理

  1. temperatureThe reaction was cooled in an ice bath
  2. filtrationfiltered
  3. dissolutionThe precipitate was dissolved in acetone (250 ml)
  4. additionThe resulting solution was treated with charcoal
  5. temperatureat reflux
  6. filtrationfiltered through a pad of silica gel and celite
  7. concentrationpartially concentrated
  8. customCrystals formed which
  9. filtrationwere filtered
  10. customdried