Some common heterocyclic compound, 25808-30-4, name is 2-(Methylamino)acetonitrile hydrochloride, molecular formula is C3H7ClN2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. name: 2-(Methylamino)acetonitrile hydrochloride
54.5 g of ethyl chloroformate was then poured dropwise into the resulting mix, with the temperature being maintained at between 0° and 5° to form a mixed anhydride. When the addition operation was concluded, agitation was effected for a further period of 30 minutes at 5° C. At the same time, 400 cc of chloroform and 55.5 g of triethylamine were introduced into a one liter balloon flask provided with an agitator and the mixture was cooled in an ice bath. 59 g of methylamino acetonitrile hydrochloride in finely divided form was then added gradually. The solution thus obtained was then gradually added to the solution of mixed anhydride which was produced previously, with the temperature being maintained at between 5° and 10°. At the end of the addition operation, agitation was effected for a further period of 1 hour at 5°C. The temperature of the reaction mix was permitted to rise and the reaction medium was left overnight. The chloroform was then distilled off under a slight vacuum. The residue was dissolved in water and the last traces of chloroform were removed by entrainment with water. The remaining product crystallized out. A few drops of soda lye were then added to make the medium slightly alkaline and then the product obtained was drained, washed with water until the Cl- ions were removed, and dried at 40°. Weight obtained=92 g MP=128° C. Yield=72.5percent
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 25808-30-4, its application will become more common.
Reference:
Patent; Societe d’Etudes Scientifiques et Industrielles de l’Ile-de-France; US4703055; (1987); A;,
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