反応 #417901

反応方程式

phosphoryl chloride

dibenzo[f,h]quinoxaline-1-oxide

potassium carbonate

→

2-Chloro-Dibenzo[f,h]Quinoxaline

収率 93.0%

溶媒

water

反応条件

後処理

1. 1
   その他obtained in the above Step 1
2. 2
   温度while being heated
3. 3
   温度under reflux for 1 hour
4. 4
   ろ過This solution was filtered
5. 5
   洗浄the obtained residue was washed with water
6. 6
   その他methanol to give
7. 7
   その他the object of the synthesis (as a pale yellow powder in a yield of 93%)
8. 8
   その他The synthesis scheme of Step 2

実験手順

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).

出典