반응 #1731

반응 방정식

6-hydroxynicotinic acid

sulfuric acid

benzyl alcohol

→

benzyl 6-hydroxy-nicotinate

반응 조건

후처리

1. 1
   온도at reflux for 3 days
2. 2
   추출extracted several times with ethyl acetate
3. 3
   세척washed with water
4. 4
   건조dried over sodium sulfate
5. 5
   기타evaporated, firstly in a water-jet vacuum
6. 6
   여과The semi-crystalline residue was filtered over silica gel (eluent hexane/ethyl acetate=2:1
7. 7
   기타ethyl acetate) and recrystallized from ethyl acetate/hexane

실험 절차

30 g of 6-hydroxynicotinic acid were treated with 500 ml of benzyl alcohol and 1 ml of concentrated sulfuric acid. After boiling at reflux for 3 days, the reaction mixture was poured on to ice-water, extracted several times with ethyl acetate, washed with water, dried over sodium sulfate and evaporated, firstly in a water-jet vacuum and then in a high vacuum. The semi-crystalline residue was filtered over silica gel (eluent hexane/ethyl acetate=2:1, then ethyl acetate) and recrystallized from ethyl acetate/hexane. There were obtained 19 g of benzyl 6-hydroxy-nicotinate in colourless crystals, m.p. 178°-179° C.

출처