ethyl N-carbamoylcarbamate

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 50 g (0.378 Mol) of ethylallophanate and 76.6 g (0.416 Mol) of 1,2-diphenylhydrazine were suspended in 100 ml of anhydrous xylene and refluxed for 6 hours with stirring, during which time ammonia was released. The solvent was distilled off, the residue was mixed with 150 ml of xylene once more and refluxed for 1 hour. The mixture was left to cool, the reaction product was suction filtered, and thoroughly washed with cold xylene. After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained, mp. 216°-217° C. refluxed for 6 hours The solvent was distilled off the residue was mixed with 150 ml of xylene once more refluxed for 1 hour The mixture was left to cool filtered thoroughly washed with cold xylene After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 50 g (0.378 Mol) of ethylallophanate and 76.6 g (0.416 Mol) of 1,2-diphenylhydrazine were suspended in 100 ml of anhydrous xylene and refluxed for 6 hours with stirring, during which time ammonia was released. The solvent was distilled off, the residue was mixed with 150 ml of xylene once more and refluxed for 1 hour. The mixture was left to cool, the reaction product was suction filtered, and thoroughly washed with cold xylene. After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained, mp. 216°-217° C. refluxed for 6 hours The solvent was distilled off the residue was mixed with 150 ml of xylene once more refluxed for 1 hour The mixture was left to cool filtered thoroughly washed with cold xylene After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 50 g (0.378 Mol) of ethylallophanate and 76.6 g (0.416 Mol) of 1,2-diphenylhydrazine were suspended in 100 ml of anhydrous xylene and refluxed for 6 hours with stirring, during which time ammonia was released. The solvent was distilled off, the residue was mixed with 150 ml of xylene once more and refluxed for 1 hour. The mixture was left to cool, the reaction product was suction filtered, and thoroughly washed with cold xylene. After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained, mp. 216°-217° C. refluxed for 6 hours The solvent was distilled off the residue was mixed with 150 ml of xylene once more refluxed for 1 hour The mixture was left to cool filtered thoroughly washed with cold xylene After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 50 g (0.378 Mol) of ethylallophanate and 76.6 g (0.416 Mol) of 1,2-diphenylhydrazine were suspended in 100 ml of anhydrous xylene and refluxed for 6 hours with stirring, during which time ammonia was released. The solvent was distilled off, the residue was mixed with 150 ml of xylene once more and refluxed for 1 hour. The mixture was left to cool, the reaction product was suction filtered, and thoroughly washed with cold xylene. After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained, mp. 216°-217° C. refluxed for 6 hours The solvent was distilled off the residue was mixed with 150 ml of xylene once more refluxed for 1 hour The mixture was left to cool filtered thoroughly washed with cold xylene After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 50 g (0.378 Mol) of ethylallophanate and 76.6 g (0.416 Mol) of 1,2-diphenylhydrazine were suspended in 100 ml of anhydrous xylene and refluxed for 6 hours with stirring, during which time ammonia was released. The solvent was distilled off, the residue was mixed with 150 ml of xylene once more and refluxed for 1 hour. The mixture was left to cool, the reaction product was suction filtered, and thoroughly washed with cold xylene. After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained, mp. 216°-217° C. refluxed for 6 hours The solvent was distilled off the residue was mixed with 150 ml of xylene once more refluxed for 1 hour The mixture was left to cool filtered thoroughly washed with cold xylene After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 50 g (0.378 Mol) of ethylallophanate and 76.6 g (0.416 Mol) of 1,2-diphenylhydrazine were suspended in 100 ml of anhydrous xylene and refluxed for 6 hours with stirring, during which time ammonia was released. The solvent was distilled off, the residue was mixed with 150 ml of xylene once more and refluxed for 1 hour. The mixture was left to cool, the reaction product was suction filtered, and thoroughly washed with cold xylene. After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained, mp. 216°-217° C. refluxed for 6 hours The solvent was distilled off the residue was mixed with 150 ml of xylene once more refluxed for 1 hour The mixture was left to cool filtered thoroughly washed with cold xylene After drying in vacuo, 60.0 g (63% of theory) of colourless crystals were obtained

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 0.65 ml (0.72 g, 0.00443 moles) of ethyl pyrocarbonate are added to a solution of 1.0 g (0.00285 moles) of 1-(1',3'-bis/2",6"-dimethylphenyl/-4'-methyl-imidazolidine-2'-ylidene)-urea, prepared as described in Example 72, in 10 ml of dry chloroform, and the mixture is allowed to stand at room temperature for 48 hours. Thereafter the solvent and the excess of the reactant are distilled off under reduced pressure. The oily residue is dissolved in 10 ml of diethyl ether, the insolubles are filtered off, and the filtrate is concentrated to a final volume of about 2 ml. Next day the separated crystalline product is filtered off, washed with a small amount of diethyl ether and dried. 0.5 g (41.7%) of 1-(1',3'-bis/2",6"-dimethylphenyl/-4'-methyl-imidazolidine-2'-ylidene)-3-carbethoxy-urea are obtained; m.p.: 123°-125° C. prepared Thereafter the solvent and the excess of the reactant are distilled off under reduced pressure The oily residue is dissolved in 10 ml of diethyl ether the insolubles are filtered off the filtrate is concentrated to a final volume of about 2 ml Next day the separated crystalline product is filtered off washed with a small amount of diethyl ether dried