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The 3 (4),7(8) -dihydroxymethylbicyclo[4 .3 .0]nonane obtained after the hydrogenation of 3(4),7(8)-bisformylbicyclo[4.3.0]nonane and subsequent distillation Was introduced into the alkali melt. 184.3 g of the diol Were initially charged together With 12.0 g of acetic acid in a 1 liter autoclave and admixed With 57.6 g of NaOH (solid, pure) and 62.6 g of KOH (solid, 85%). The mixture Was heated to 250° C. With stirring, in the course of Which the pressure Was regulated to 2 MPa. After 2 hours at 250° C., the temperature Was increased to 280° C.; the pressure remained at 2 MPa. After a reaction time of 2 hours at 280° C., the mixture Was cooled, While Water Was pumped in an amount of 300 g at about 160° C. The resulting solution Was admixed With 185.0 g of toluene and acidi?ed by adding 1,813 g of 20% aqueous sulfuric acid. The organic phase Was subsequently extracted ?ve times With 300.0 g of Water. After the solvent had been distilled off, the desired dicarboxylic acid Was obtained as a solid in the distillation residue. The Weight of bicyclo[4.3.0]nonane-3(4),7(8)-dicarboxylic acid Was 197.1g at a purity of 99.07%.Код: Выделить всё
300 grams of tricyclodecane-dimethylol having the and 210 grams potassium hydroxide were placed in an autoclave of 2.5 liters capacity. After having sealed the autoclave, the air was removed by passing through nitrogen. Then the autoclave was heated to 250° C. and maintained at this temperature for 20 minutes. Under these conditions, the pressure in the autoclave increased to 110 kg./ sq. cm. corresponding to 125 normal liters of hydrogen split off. After cooling, the hydrogen was released and the reaction mixture was removed from the autoclave.Код: Выделить всё
http://www.google.com/patents/US7358385
http://www.google.com/patents/US2841614
