반응 #417901

반응 방정식

phosphoryl chloride

dibenzo[f,h]quinoxaline-1-oxide

potassium carbonate

→

2-Chloro-Dibenzo[f,h]Quinoxaline

수율 93.0%

용매

water

반응 조건

후처리

1. 1
   기타obtained in the above Step 1
2. 2
   온도while being heated
3. 3
   온도under reflux for 1 hour
4. 4
   여과This solution was filtered
5. 5
   세척the obtained residue was washed with water
6. 6
   기타methanol to give
7. 7
   기타the object of the synthesis (as a pale yellow powder in a yield of 93%)
8. 8
   기타The synthesis scheme of Step 2

실험 절차

Next, 18 mL of phosphoryl chloride was dripped into 2.91 g of dibenzo[f,h]quinoxaline-1-oxide obtained in the above Step 1. This mixed solution was stirred while being heated under reflux for 1 hour. This mixed solution was poured into iced water, followed by addition of potassium carbonate so that the mixture was alkaline. This solution was filtered, and the obtained residue was washed with water and then methanol to give the object of the synthesis (as a pale yellow powder in a yield of 93%). The synthesis scheme of Step 2 is illustrated in the following (a″′-2-2).

출처