반응 #790929

반응 방정식

potassium hydroxide

glycerol

3,4-methylenedioxynitrobenzene

water

→

1-(2-hydroxy-4-nitrophenoxy)propane-2,3-diol

반응 조건

후처리

1. 1
   여과The mixture is filtered in order
2. 2
   기타to remove a small quantity of starting material
3. 3
   workup.ADDITIONtreated with 10 g of vegetable charcoal
4. 4
   workup.STIRRINGAfter stirring for a few minutes at ambient temperature
5. 5
   기타removal of the vegetable charcoal
6. 6
   여과by filtration
7. 7
   workup.WAITthe solution is left
8. 8
   기타the expected product which has crystallized
9. 9
   여과is then filtered off
10. 10
    기타After recrystallization from ethanol
11. 11
    기타drying in vacuo

실험 절차

0.3 mol (19.8 g) of 85% by weight potassium hydroxide pellets is dissolved in 210 ml of glycerol, and 0.25 mol (41.75 g) of 3,4-methylenedioxynitrobenzene is then added, with stirring. After heating for one and a half hours in the region of 110° C., the reaction medium is poured into 1.5 liters of iced water. The mixture is filtered in order to remove a small quantity of starting material. The filtrate is acidified to pH=4 with hydrochloric acid and then treated with 10 g of vegetable charcoal. After stirring for a few minutes at ambient temperature and removal of the vegetable charcoal by filtration, the solution is left to stand overnight at 0° C. and the expected product which has crystallized is then filtered off. After recrystallization from ethanol and drying in vacuo, the product melts at 148° C.

출처