HRID907471

反应详情

EQUATION

反应方程式

HRID 907471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture containing 5,9-bis(2,2,2-trifluoroethoxy)furo[3,4-g]quinoline-6,8-dione (42 g, 106 mmol) 5 and 1-(4-amino-3-methylphenyl)methanesulfonamide 15 (24 g, 1.13 equiv) from Preparative Example 1 in AcOH (350 ml) was degassed under vacuum and heated to reflux under nitrogen for 6.5 h. The solvent was then evaporated and the residue was partially dissolved into 50% EtOAc/toluene (800 ml) and cooled down to 0 C. The solid was filtered and washed with toluene to yield a first crop of material as a brownish solid (50.36 g).

WORKUP

后处理

  1. customwas degassed under vacuum
  2. temperatureheated
  3. temperatureto reflux under nitrogen for 6.5 h
  4. customThe solvent was then evaporated
  5. dissolutionthe residue was partially dissolved into 50% EtOAc/toluene (800 ml)
  6. temperaturecooled down to 0 C
  7. filtrationThe solid was filtered
  8. washwashed with toluene