반응 #1161493

반응 방정식

3,4-methylenedioxynitrobenzene

ammonia

diethylene glycol dimethyl ether

→

expected product

2-amino-5-nitrophenol

용매

water

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   기타The unreacted initial product precipitates
3. 3
   여과It is recovered by filtration
4. 4
   여과After filtration
5. 5
   추출the filtrate is extracted with ethyl acetate
6. 6
   workup.ADDITIONThe residue is treated with 25 ml of acetic anhydride
7. 7
   온도After cooling

실험 절차

A solution of 0.18 mol (30 g) of 3,4-methylenedioxynitrobenzene in a mixture of 240 ml of 28% strength ammonia solution and 240 ml of diethylene glycol dimethyl ether is heated at 100° C. for 28 hours in an autoclave. After cooling, 480 ml of water are added. The unreacted initial product precipitates. It is recovered by filtration and the filtrate is then neutralised with hydrochloric acid. After filtration, the filtrate is extracted with ethyl acetate. The ethyl acetate is driven off in vacuo. The residue is treated with 25 ml of acetic anhydride and then kept in a boiling water-bath for 30 minutes. After cooling, the expected product is isolated in the form of the acetyl derivative. This acetyl derivative is hydrolysed with 45 ml of hydrochloric acid of density 1.17, at 90° C. for one hour. After dilution and neutralisation of the solution containing hydrochloric acid, 2-amino-5-nitrophenol is isolated by filtration. Melting point=207° C.

출처