Reaktion #417901

Reaktionsgleichung

phosphoryl chloride

dibenzo[f,h]quinoxaline-1-oxide

potassium carbonate

→

2-Chloro-Dibenzo[f,h]Quinoxaline

Ausbeute 93.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeobtained in the above Step 1
2. 2
   Temperaturwhile being heated
3. 3
   Temperaturunder reflux for 1 hour
4. 4
   FiltrationThis solution was filtered
5. 5
   Waschenthe obtained residue was washed with water
6. 6
   Sonstigemethanol to give
7. 7
   Sonstigethe object of the synthesis (as a pale yellow powder in a yield of 93%)
8. 8
   SonstigeThe synthesis scheme of Step 2

Vorschrift

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).

Quelle