2-amino-2,4-dimethylpentanenitrile

Conditions: temp:15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In the same manner as in Example 1, 2-amino-2,4-dimethylpentanonitrile and sodium hypochlorite were reacted. By iodometry, it was found that the total oxidative compounds in both the water and ethyl acetate phases after reaction was 0.05 equivalent. The reaction mixture was adjusted to a pH of 6 with a dilute sulfuric acid, and a solution of 6.5 g (0.125 equivalent) of sodium bisulfite in 30 ml of water was added thereto. The resulting mixture was stirred at 15° C. for 30 minutes to effect the reduction. Thereafter, the ethyl acetate phase was separated from the water phase, and the ethyl acetate in the organic phase was removed by distillation. Water was added to the residue and precipitated white crystals were filtered, washed with water and dried to obtain 26.0 g of 2,2'-azobis(2,4-dimethylvaleronitrile). Yield was 89 mole %. The product was analyzed by iodometry, and it was found that the amount of oxidative impurities was 100 ppm or less and that the purity of the product was 99.5%. after reaction Thereafter, the ethyl acetate phase was separated from the water phase the ethyl acetate in the organic phase was removed by distillation Water was added to the residue precipitated white crystals were filtered washed with water dried

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

Procedure: Next, 213 g of a 10% aqueous sodium hypochlorite solution was cooled to 5° C. and 0.5 g of benzyltriethylammonium chloride was added thereto. To the resulting aqueous solution was added 200 ml of an ethyl acetate solution containing 33 g of the resulting 90%-pure 2-amino-2,4-dimethylpentanonitrile over 30 minutes with stirring. This reaction mixture was stirred at 5° to 10° C. for 3 hours, and the organic and water phases were separated from each other. Ethyl acetate was removed from the organic phase under reduced pressure. The resulting white crystals were washed with water and dried to obtain 24.8 g of 2,2'-azobis(2,4-dimethylpentanonitrile). Yield was 85 mole %. This reaction mixture was stirred at 5° to 10° C. for 3 hours the organic and water phases were separated from each other Ethyl acetate was removed from the organic phase under reduced pressure The resulting white crystals were washed with water dried

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

Procedure: To a 1-liter autoclave were added 7 moles of ammonia and then 3.5 moles of 90%-pure 2-hydroxy-2,4-dimethylpentanonitrile, and the mixture was reacted at 27° C. for 10 hours at a rate of 300 r.p.m. Thus, 2-amino-2,4-dimethylpentanonitrile was synthesized. After reaction, the reaction mixture was taken out of the autoclave, and 44 g of the water phase was separated. The residue was distilled in a wetted wall tower under the following conditions: Temperature of the heating portion 25° C.; pressure 30 mmHg; and residence time in the heating portion 1 minute or less. Low-boiling compounds were thus distilled off and purified 2-amino-2,4-dimethylpentanonitrile was withdrawn from the bottom. The yield of the purified product was 90.0 mole % based on cyanohydrin. This purified product contained 0.5% by weight of ammonia and 0.8% by weight of hydrogen cyanide, and its purity was 90%. After reaction was separated The residue was distilled in a wetted wall tower under the following conditions Temperature of the heating portion 25° C. in the heating portion 1 minute or less were thus distilled off purified 2-amino-2,4-dimethylpentanonitrile was withdrawn from the bottom

Conditions: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a solution of 63.2 parts of 2-amino-2,4-dimethylpentanonitrile in 592 parts of methanol are added over a 20 minute period at -10°C. with agitation 377 parts of a 15% aqueous sodium hypochlorite solution. The reaction was then allowed to warm to 10°C. and held for 10 minutes. At this point methanol constitutes 74 volume percent of the aqueous solvent. The resulting reaction product was diluted with 500 parts of water and titrated with standard sodium thiosulfate as described in Example 1. About 0.015 equivalent of oxidizing agent was present. The resulting slurry was then acidified to a pH of 1.0 with 15% hydrochloric acid and 0.52 gram of sodium nitrite (0.015 equivalent) were stirred into the mixture. The precipitated 2,2'-azobis (2,4-dimethylvaleronitrile) was isolated by filtration and found to be non-oily, white and dry with a purity of 98%. The resulting reaction product