反应详情

A stirred mixture of 6.9 g (0.035 mole) of p-trifluoromethylbenzylamine hydrochloride and 4.3 (0.035 mole) of 1-i-propyl-3-cyanoguanidine is immersed in a 180° C oil bath for 1 hour. The melt is cooled and dissolved in 35 ml of hot water. The solution is cooled in an ice bath, made alkaline with 40% sodium hydroxide solution, and extracted with 150 ml of ether. The ether layer is dried over potassium carbonate, filtered and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid solution. The precipitate is washed twice with 25 ml of anhydrous ether and recrystallized from a mixture of ethanol and heptane (3:5) to obtain 1-(p-trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride.

1. customis immersed in a 180° C
2. customfor 1 hour
3. temperatureThe melt is cooled
4. temperatureThe solution is cooled in an ice bath
5. extractionextracted with 150 ml of ether
6. dry with materialThe ether layer is dried over potassium carbonate
7. filtrationfiltered
8. washThe precipitate is washed twice with 25 ml of anhydrous ether
9. customrecrystallized from a mixture of ethanol and heptane (3:5)