반응 #790927

반응 방정식

3,4-methylenedioxynitrobenzene

N-acetylethanolamine

→

N-(2-hydroxy-4-nitrophenoxyethyl)acetamide

반응 조건

후처리

1. 1
   온도After heating for one hour
2. 2
   workup.STIRRINGthe reaction medium is stirred at 100° C. for a further 3 hours
3. 3
   여과is filtered off
4. 4
   기타to precipitate the expected product
5. 5
   여과It is filtered off
6. 6
   세척washed with water
7. 7
   기타dried in vacuo

실험 절차

0.05 mol (8.35 g) of 3,4-methylenedioxynitrobenzene is introduced into 42 ml of N-acetylethanolamine. The mixture is heated to the region of 100° C., with stirring, and 0.055 mol (3.7 ml) of 15N potassium hydroxide solution is then added. After heating for one hour, 0.050 mol (3.3 ml) of 15N potassium hydroxide solution is added and the reaction medium is stirred at 100° C. for a further 3 hours and then poured onto 120 g of crushed ice. The unreacted starting material, which is insoluble in an alkaline medium, is filtered off. The filtrate is then acidified to pH=5.6 with hydrochloric acid in order to precipitate the expected product. It is filtered off, washed with water and dried in vacuo. It melts at 165° C.

출처