반응 #6290

반응 방정식

vanillin

1,10-dibromodecane

potassium carbonate

acetone

→

compound

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

용매

water

반응 조건

후처리

1. 1
   온도cooled
2. 2
   workup.DISSOLUTIONAfter the salts had dissolved
3. 3
   여과The solid product was filtered
4. 4
   세척washed twice with water
5. 5
   기타recrystallized (still wet) from 250 ml of ethanol
6. 6
   온도Cooling to 25° C.

실험 절차

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.

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