反应 #417900

反应方程式

3-chlorobenzoic acid

Water

dibenzo[f,h]quinoxaline

→

Dibenzo[f,h]quinoxaline-1-oxide

收率 51.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   萃取the organic layer was extracted with dichloromethane
2. 2
   洗涤The obtained organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   过滤Then, the resulting solution was filtered
5. 5
   workup.DISTILLATIONThe solvent of this solution was distilled off
6. 6
   其他The resulting residue was purified by silica gel column chromatography which
7. 7
   其他By recrystallization from dichloromethane
8. 8
   其他the object of the synthesis was obtained (as a white powder in a yield of 51%)
9. 9
   其他The synthesis scheme of Step 1

实验过程

First, to a solution in which 1.36 g of dibenzo[f,h]quinoxaline was dissolved in 20 mL of dichloromethane was added 2.04 g of 3-chlorobenzoic acid (abbreviation: MCPBA) in a nitrogen atmosphere, followed by stirring at room temperature for 1 week. Water was added to this mixture, and the organic layer was extracted with dichloromethane. The obtained organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. Then, the resulting solution was filtered. The solvent of this solution was distilled off. The resulting residue was purified by silica gel column chromatography which uses a mixed solvent of dichloromethane and ethyl acetate as a developing layer. By recrystallization from dichloromethane, the object of the synthesis was obtained (as a white powder in a yield of 51%). The synthesis scheme of Step 1 is illustrated in the following (a″′-2-1).

来源