HRID907471
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas degassed under vacuum
- temperatureheated
- temperatureto reflux under nitrogen for 6.5 h
- customThe solvent was then evaporated
- dissolutionthe residue was partially dissolved into 50% EtOAc/toluene (800 ml)
- temperaturecooled down to 0 C
- filtrationThe solid was filtered
- washwashed with toluene