摘要 |
The prepn. of nitrobbibenzyls (nitro substit. 1,2 diphenyl ethanes) by air oxidn. using metal-tetra-phenyl-porphin catalyst and a poly-ethylene-glycol as catalyst in an alkaline organic solvent is new and gives higher yield. - The metal is pref. Mn. The poly-ethylene-glycol may be PEG 200,300,400,1000 but is pref. PEG 600. The solvent is pref. an alcohol, but may also be di methylsulphoxide. The prepn. of o-nitrobibenzyl from o-nitro-toluene is partic. claimed. - In an example to 33% KOH in methanol was added a catalytic quantity of manganese tetra-phenyl-porphin chloride. the mixt. was cooled to 25 deg.C and 13.7g, 0.1 mole of o-nitrotoluene added. Air was passed for 6 hrs. at 25 deg.C 150 ml. water and 50 ml. methanol were added and the result was filtered. Recryst from ethanol gave 55-65% yield of m.pt. 120-121 deg.C. (Provisional Basic previously advised in week 8851).(0/0) |