2,6-DIMETHYLCYCLOHEXYLAMINE

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: trans-2-ethylcyclohexylamine, B.P. 77°-78° (23 mm.); 2,6-diethylcyclohexylamine, B.P. 96° C., (17 mm.);

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1,650 parts by weight of 2,6-dimethylphenol and 150 parts by weight of a pulverulent catalyst containing 10.0% by weight of palladium and 5.0% by weight of praseodymium oxide on aluminum oxide were introduced into a stirred autoclave having a capacity of 10,000 parts by volume. The autoclave was closed and 1,370 parts by weight of ammonia were forced in. The autoclave was then heated to 250° C. and hydrogen was introduced to bring the pressure to 300 bar. The autoclave was kept at the reaction temperature until constant pressure was achieved (about 10 hours). It was then allowed to cool and the mixture was filtered to give 1,691 parts by weight (98.5%) of 2,6-dimethylcyclohexylamine which, according to gas chromatography and NMR analysis, had the following isomer distribution: were introduced into a stirred autoclave The autoclave was closed (about 10 hours) to cool the mixture was filtered

反应条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1,650 parts by weight of 2,6-dimethylphenol and 150 parts by weight of a pulverulent catalyst containing 10.0% by weight of palladium and 5.0% by weight of praseodymium oxide on aluminum oxide were introduced into a stirred autoclave having a capacity of 10,000 parts by volume. The autoclave was closed and 1,370 parts by weight of ammonia were forced in. The autoclave was then heated to 250° C. and hydrogen was introduced to bring the pressure to 300 bar. The autoclave was kept at the reaction temperature until constant pressure was achieved (about 10 hours). It was then allowed to cool and the mixture was filtered to give 1,691 parts by weight (98.5%) of 2,6-dimethylcyclohexylamine which, according to gas chromatography and NMR analysis, had the following isomer distribution: were introduced into a stirred autoclave The autoclave was closed (about 10 hours) to cool the mixture was filtered

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A catalyst consisting of 1.0% by weight of palladium and 0.5% by weight of praseodymium oxide, the remainder being aluminum oxide, in extrudate form is introduced into a 1 l cylindrical reaction tube and is heated to 200° C. A mixture of 60 g of 2,6-dimethylphenol and 360 g of liquid ammonia per hour is passed over this catalyst bed. At the same time, 100 liters (S.T.P.) of hydrogen are passed in co-current through the reaction tube under a pressure of 200 bar. The reaction product which leaves the tube is cooled under superatmospheric pressure and is then let down. About 62 g of crude product, which gives 60 g of pure 2,6-dimethylcyclohexylamine (corresponding to a yield of 96%) on distillation, are thereby obtained per hour. in extrudate form is introduced into a 1 l cylindrical reaction tube The reaction product which leaves the tube is cooled under superatmospheric pressure

反应条件: temp:230.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.650 kg of 2,6-dimethylphenol and 150 g of a pulverulent catalyst which contains 5.0% by weight of palladium and 2.5% by weight of praseodymium oxide, the remainder being aluminum oxide, are introduced into a 10 l stirred autoclave. The autoclave is closed and 1.370 kg of ammonia are forced in. The mixture is then heated to 230° C. and a pressure of 200 bar is established by forcing in hydrogen. The mixture is kept at the reaction temperature until a constant pressure is achieved (about 8 hours). It is then left to cool, and is filtered to give 1.710 kg of crude 2,6-dimethylcyclohexylamine (a mixture of 3 stereoisomeric 2,6-dimethylcyclohexylamines). The crude product is distilled to give 1.685 kg of 2,6-dimethylcyclohexylamine, boiling point=167°-168° C., corresponding to a yield of 98%. are introduced into a 10 l The autoclave is closed (about 8 hours) It is then left to cool is filtered

反应条件: temp:230.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.650 kg of 2,6-dimethylphenol and 150 g of a pulverulent catalyst which contains 5.0% by weight of palladium and 2.5% by weight of praseodymium oxide, the remainder being aluminum oxide, are introduced into a 10 l stirred autoclave. The autoclave is closed and 1.370 kg of ammonia are forced in. The mixture is then heated to 230° C. and a pressure of 200 bar is established by forcing in hydrogen. The mixture is kept at the reaction temperature until a constant pressure is achieved (about 8 hours). It is then left to cool, and is filtered to give 1.710 kg of crude 2,6-dimethylcyclohexylamine (a mixture of 3 stereoisomeric 2,6-dimethylcyclohexylamines). The crude product is distilled to give 1.685 kg of 2,6-dimethylcyclohexylamine, boiling point=167°-168° C., corresponding to a yield of 98%. are introduced into a 10 l The autoclave is closed (about 8 hours) It is then left to cool is filtered

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: contacting said 3,5-dimethyl-4-nitro-cyclohexene with hydrogen at a temperature of about 0° C. to about 200° C. and a pressure of about 0 psig to about 1500 psig in the presence of a palladium catalyst to form 2,6-dimethylcyclohexyl amine; and at a temperature of about 0° C. to about 200° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The thus formed oxime is thereafter reduced in the presence of a Na--alcohol couple to 2,6-dimethylcyclohexylamine at a temperature in the range 0° to 80° C. at 1-5 atmospheres pressure: ##STR10## Amine is then dissolved in o-dichlorobenzene and in the presence of excess phosgene with the reaction being performed in two temperature stages with the first temperature stage in the range -20° to 20° C. and the second from 20° to 200° C. with pressures ranging from 1 to 15 atmospheres to form 2,6-dimethylcyclohexylisocyanate, thusly: ##STR11## being performed in two temperature stages with the first temperature stage in the range -20° to 20° C. second from 20° to 200° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: trans-2-ethylcyclohexylamine, B.P. 77°-78° (23 mm.); 2,6-diethylcyclohexylamine, B.P. 96° C., (17 mm.);