3-(3-Pyridinyloxy)-1-nitrobenzene synthesis
- Product Name:3-(3-Pyridinyloxy)-1-nitrobenzene
- CAS Number:28232-52-2
- Molecular formula:C11H8N2O3
- Molecular Weight:216.19
Yield:28232-52-2 86%
Reaction Conditions:
with potassium carbonate in DMF (N,N-dimethyl-formamide) at 150; for 16 h;
Steps:
a 3- (3-PYRIDINYLOXY) PHENYLAMINE
a) 50 g (0.53 mol) of 3-HYDROXYPYRIDINE, 178. 8 g (1.05 mol) of 1,3- dinitrobenzene and 159.9 g (1.16 mol) of K2C03 WERE suspended in 1.4 1 of DMF, and the suspension was heated to 150°C. After the reaction mixture had been stirred at 150°C for 16 hours, it was cooled to room temperature and evaporated. The residue was taken up in 1.5 1 of ethyl acetate, stirred for 30 minutes and filtered. The filtrate was extracted with 10% HCI solution. The aqueous phase was rendered alkaline using NH40H solution and extracted with ethyl acetate. The combined organic phases were dried using NA2SO4, filtered and evaporated. The residue was purified by column chromatography (1 kg of silica gel, eluent : dichloromethane), taken up in 10% HCI solution and extracted with ethyl acetate. The aqueous phase was rendered alkaline using NH40H solution and extracted with ethyl acetate. The organic phase was dried using NA2SO4, filtered and evaporated. Yield : 98 g (86%) of 7, brown oil
References:
WO2004/85399,2004,A1 Location in patent:Page 168; 169
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