HRID568366

反应详情

EQUATION

反应方程式

HRID 568366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 6-[3,5-dimethyl-1,2,4-triazol-4-yl]-2-methoxy-8-methylquinoline (0.24 g) in 5M hydrochloric acid (20 cm3) was heated under reflux for 1 hour. The cooled solution was then basified to pH8 with 10% aqueous sodium carbonate solution and extracted with chloroform (5×50 cm3). The combined and dried (MgSO4) organic phases were evaporated in vacuo and the residue was chromatographed on silica (Merck "MK 60.9385" [Trade Mark]) eluting with dichloromethane:methanol, 20:1, to afford 6-[3,5-dimethyl-1,2,4-triazol-4-yl]-8-methyl-2-(1H)-quinolone, 0.66H2O, m.p. 308°-310° (0.17 g).

WORKUP

后处理

  1. temperatureunder reflux for 1 hour
  2. extractionextracted with chloroform (5×50 cm3)
  3. dry with materialdried (MgSO4) organic phases
  4. customwere evaporated in vacuo
  5. customthe residue was chromatographed on silica (Merck "MK 60.9385" [Trade Mark])
  6. washeluting with dichloromethane