تفاعل #6290

معادلة التفاعل

vanillin

1,10-dibromodecane

potassium carbonate

acetone

→

compound

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

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled
2. 2
   workup.DISSOLUTIONAfter the salts had dissolved
3. 3
   ترشيحThe solid product was filtered
4. 4
   غسيلwashed twice with water
5. 5
   أخرىrecrystallized (still wet) from 250 ml of ethanol
6. 6
   درجة الحرارةCooling to 25° C.

الإجراء التجريبي

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.

المصدر