反応 #460004

反応方程式

4-phenoxy-phenol

2-chloroethyl-vinyl ether

4-phenoxy-phenol

4-phenoxy-phenol

→

1-(2-chloroethoxy)-1-[(4-phenoxy)-phenoxy]-ethane

溶媒

diethyl ether

反応条件

後処理

1. 1
   workup.ADDITIONan addition
2. 2
   その他is made in portions at room temperature
3. 3
   workup.DISSOLUTIONcompletely dissolving
4. 4
   洗浄the ether solution is washed three times with 10% potassium hydroxide solution and three times with saturated sodium chloride solution
5. 5
   乾燥The ether solution is subsequently dried over sodium sulphate
6. 6
   その他the ether and the readily volatile constituents (traces of 2-chloroethyl-vinyl ether) are completely removed in vacuo

実験手順

64 g of freshly distilled 2-chloroethyl-vinyl ether is placed into a flask; one drop of concentrated hydrochloric acid is added, and thereupon an addition is made in portions at room temperature, with stirring, of 93 g of 4-phenoxy-phenol (duration of addition about 1 hour). During the addition of 4-phenoxy-phenol, the temperature rises to about 32°- 34° C, with the 4-phenoxy-phenol completely dissolving. After two further hours' stirring, the reaction mixture is diluted with 300 ml of diethyl ether; the ether solution is washed three times with 10% potassium hydroxide solution and three times with saturated sodium chloride solution. The ether solution is subsequently dried over sodium sulphate, and the ether and the readily volatile constituents (traces of 2-chloroethyl-vinyl ether) are completely removed in vacuo. There is obtained 1-(2-chloroethoxy)-1-[(4-phenoxy)-phenoxy]-ethane in the form of colorless oil having a refractive index of nD20 = 1.5516 (yield 98%).

出典