反応 #86674

反応方程式

epichlorohydrin

4-phenoxyphenol

→

4-phenoxy-O-(2-hydroxy-3-chloropropyl)phenol

溶媒

ethanol

反応条件

後処理

1. 1
   その他A four-neck flask equipped with a thermometer
2. 2
   workup.ADDITIONwas added dropwise
3. 3
   workup.WAITwas performed for 6 hours
4. 4
   workup.ADDITIONthe addition reaction

実験手順

A four-neck flask equipped with a thermometer, dropping funnel, condenser tube and stirrer was charged with 305.3 g (3.3 mol) of epichlorohydrin, and while nitrogen purging was performed, the temperature was raised to 70° C. Into the flask, 204.8 g (1.1 mol) of 4-phenoxyphenol dissolved in 1020 g of ethanol was added dropwise taking 4 hours. Further, stirring was performed for 6 hours, to complete the addition reaction, for obtaining 4-phenoxy-O-(2-hydroxy-3-chloropropyl)phenol. In succession, the temperature in the flask was lowered to 25° C., and into the flask, 229 g (2.75 mol) of 48% NaOH aqueous solution was added dropwise taking 2 hours. Further, stirring was performed for 1 hour. After completion of cyclization reaction, ethanol was distilled away, and 410 g of toluene was used for extraction, 5% saline solution being used for washing twice. Toluene and epichlorohydrin were removed from the organic layer under reduced pressure, to obtain 215.6 g of a viscous liquid (yield 89%). The purity of 4-phenoxyphenyl glycidyl ether as the main product was 92% (GCarea %).

出典