反応 #52131

反応方程式

resorcinol

cyanuric chloride

aluminum chloride

phenyl ether

→

2,4-bis(2,4-dihyroxyphenyl)-6-(4-phenoxyphenyl)-1,3,5-triazine

収率 10.1%

溶媒

o-dichlorobenzene

反応条件

後処理

1. 1
   温度gradually heated to 110-115° C.
2. 2
   その他the reaction mixture quenched with water
3. 3
   その他O-Dichlorobenzene was removed azeotropically from the product mixture
4. 4
   ろ過the precipitated material filtered
5. 5
   洗浄washed with water
6. 6
   その他The crude product was purified by column chromatography

実験手順

To a stirring mixture of 9 gm of cyanuric chloride, 20 gm of aluminum chloride in 50 mL of o-dichlorobenzene was added 8.5 gm of phenyl ether followed by 11 gm of resorcinol. The reaction mixture was first stirred at room temperature and then gradually heated to 110-115° C., and then held for 4 hr at this temperature. The heating was discontinued, and the reaction mixture quenched with water. O-Dichlorobenzene was removed azeotropically from the product mixture, the precipitated material filtered, and washed with water. The crude product was purified by column chromatography to give 2.3 gm of pure 2,4-bis(2,4-dihyroxyphenyl)-6-(4-phenoxyphenyl)-1,3,5-triazine, identified by HPLC, NMR, LC-UV and mass spectroscopy.

出典