反応 #6290

反応方程式

vanillin

1,10-dibromodecane

potassium carbonate

acetone

→

compound

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

溶媒

water

反応条件

後処理

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

実験手順

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.

出典