反应详情

In a reactor are added 4.9 g of 1-cyano-3-methyl-guanidine, 6.7 g of 3-amino-5-methyl-isoxazole hydrochloride and 1.3 ml of water. The reaction mixture is heated until dissolution is complete, after which the reaction is exothermal. After cooling, the reaction mixture is taken up into 30 ml water followed by 3 ml ammonia (d = 0.89). It is then extracted with 30 ml methylene chloride. After drying, treatment with carbon black and evaporation of the solvent, the residue is crystallized from absolute ethanol, to give 2.7 g of 1-methyl-5-(5-methyl-isoxazol-3-yl)-biguanide. M.p. (cap.) = 140° C. followed by resolidification, then 150°-151° C. with introduction at 140° C. and heating at a rate of 2° C./minute.

1. temperatureThe reaction mixture is heated until dissolution
2. temperatureAfter cooling
3. extractionIt is then extracted with 30 ml methylene chloride
4. customAfter drying
5. customtreatment with carbon black and evaporation of the solvent
6. customthe residue is crystallized from absolute ethanol