反应 #6290

反应方程式

vanillin

1,10-dibromodecane

potassium carbonate

acetone

→

compound

1,10-Di(2-methoxy-4-formylphenoxy)decane

溶剂

water

反应条件

后处理

1. 1
   温度cooled
2. 2
   workup.DISSOLUTIONAfter the salts had dissolved
3. 3
   过滤The solid product was filtered
4. 4
   洗涤washed twice with water
5. 5
   其他recrystallized (still wet) from 250 ml of ethanol
6. 6
   温度Cooling to 25° C.

实验过程

A slurry of 13.42 g of vanillin, 11.99 g of 1,10-dibromodecane, 6.16 g of anhydrous potassium carbonate and 300 ml of acetone was refluxed with stirring for 48 h, cooled and diluted with 400 ml of water. After the salts had dissolved, the mixture was chilled overnight at 5° C. The solid product was filtered, washed twice with water and recrystallized (still wet) from 250 ml of ethanol. Cooling to 25° C. gave 4.75 g of compound mp 93°-102° C., wetting at 65° C. (Further cooling of the mother liquors to 5° C. furnished 3.5 g of very impure materials, mp 55°-65° C.). Another recrystallization from 130 ml of ethanol raised the mp to 103°-105° C., slight wetting at 99° C.; 3.16 g.

来源