تفاعل #417900

معادلة التفاعل

3-chlorobenzoic acid

Water

dibenzo[f,h]quinoxaline

→

Dibenzo[f,h]quinoxaline-1-oxide

المردود 51.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe organic layer was extracted with dichloromethane
2. 2
   غسيلThe obtained organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution
3. 3
   تجفيفdried over anhydrous magnesium sulfate
4. 4
   ترشيحThen, the resulting solution was filtered
5. 5
   workup.DISTILLATIONThe solvent of this solution was distilled off
6. 6
   أخرىThe resulting residue was purified by silica gel column chromatography which
7. 7
   أخرىBy recrystallization from dichloromethane
8. 8
   أخرىthe object of the synthesis was obtained (as a white powder in a yield of 51%)
9. 9
   أخرىThe synthesis scheme of Step 1

الإجراء التجريبي

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).

المصدر