반응 #5851

반응 방정식

4-(10-bromodecyloxy)-4'-dodecylazobenzene

dimethylethanolamine

tetrahydrofuran

→

10-[4-[[4-(dodecyl)phenyl]azo]phenoxy]-N-(2-hvdroxyethyl)-N,N-dimethyl-1-decanaminium bromide

용매

methanol

반응 조건

후처리

1. 1
   기타A 3000 ml three-necked round bottom flask was equipped with magnetic stirring
2. 2
   온도to reflux for 24 hours
3. 3
   온도chilled in an icewater bath
4. 4
   기타The crystalline solid was isolated by suction filtration
5. 5
   여과filtered
6. 6
   기타to remove insoluble impurities
7. 7
   기타The methanol was removed by evaporation at reduced pressure The crude product
8. 8
   기타was recrystallized from tetrahydrofuran

실험 절차

A 3000 ml three-necked round bottom flask was equipped with magnetic stirring, a heating mantle, a reflux condenser, and a nitrogen atmosphere. The flask was charged with 4-(10-bromodecyloxy)-4'-dodecylazobenzene (40 g, 0.068 mol), dimethylethanolamine (95.2 g, 1.068 mole) and 1050 ml of tetrahydrofuran. The reaction mixture was allowed to reflux for 24 hours. During the course of the reaction mixture. After 24 hours, the reaction mixture was cooled to room temperature, and then chilled in an icewater bath. The crystalline solid was isolated by suction filtration. The crude product was dissolved in hot methanol and filtered to remove insoluble impurities. The methanol was removed by evaporation at reduced pressure The crude product was recrystallized from tetrahydrofuran. Yield 28.0 g, 61.0%.

출처