2,4'-DINITRODIPHENYLMETHANE synthesis
- Product Name:2,4'-DINITRODIPHENYLMETHANE
- CAS Number:1817-75-0
- Molecular formula:C13H10N2O4
- Molecular Weight:258.23
Yield:-
Reaction Conditions:
with (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride;sodium carbonate in water;toluene at 90; for 3 h;Inert atmosphere;Suzuki Coupling;
Steps:
3
In a nitrogen atmosphere, 2-nitrobenzyl bromide (A-1) (101.5 g, 0.47 mol, 1.0 eq.) and p-nitrophenylboronic acid(A-2) (86.8 g, 0.52 mol, 1.1 eq.) was added to a mixed solvent of toluene (1.5 L) and water (400 mL). Then add carbonSodium (99.6 g, 0.94 mol, 2.0 eq.), Pd(dppf)Cl2 (6.9 g, 9.4 mmol, 0.02 eq.). The reaction was performed at 90 °C for 3 h.The reaction solution was cooled and poured into water (1 L) and partitioned. The aqueous phase was then extracted with ethyl acetate (600 mL*3). Organic mergerPhase, backwash with saturated saline (400 mL*2). The organic phases are combined, dried and concentrated. The crude product was column chromatographed to obtain 2,4'-diphenylamine.Alkane dinitro (5) (77.5 g, 0.3 mol), yield 64%. (Note: contains some of the by-product 4,4'-dinitrobiphenyl, polarity andCompound 5 is consistent and cannot be separated, and recrystallization cannot be purified either).
References:
CN107814722,2018,A Location in patent:Paragraph 0047-0049
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