反应详情

A stirred mixture of 15.5 g (0.0687 mole) of α-methyl-p-trifluoromethylbenzylamine hydrochloride and 9.55 g (0.0756 mole) of 1-i-propyl-3-cyanoguanidine is immersed in a 190° C oil bath for ten minutes. The melt is cooled to room temperature, dissolved in 100 ml of water, made alkaline with 40% sodium hydroxide solution and extracted twice with 200 ml of ether. The combined ether extracts are dried over potassium carbonate, filtered, and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid ether solution. The precipitate is collected on a filter, washed twice with 50 ml of anhydrous ether, and dried at 40°C/125 mm. for 5 hours. The dihydrochloride is dissolved in 50 ml of water, made strongly alkaline with 40% sodium hydroxide solution, and extracted twice with 100 ml of ether. The combined ether extracts are dried over potassium carbonate, filtered, and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid solution. The precipitate is collected on a filter, washed twice with 50 ml of anhydrous ether, and dried at 40° C/125 mm. to obtain 1-(α-methyl-p-trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride.

1. customis immersed in a 190° C
2. customfor ten minutes
3. extractionextracted twice with 200 ml of ether
4. dry with materialThe combined ether extracts are dried over potassium carbonate
5. filtrationfiltered
6. customThe precipitate is collected on a filter
7. washwashed twice with 50 ml of anhydrous ether
8. customdried at 40°C/125 mm
9. dissolutionThe dihydrochloride is dissolved in 50 ml of water
10. extractionextracted twice with 100 ml of ether
11. dry with materialThe combined ether extracts are dried over potassium carbonate
12. filtrationfiltered
13. customThe precipitate is collected on a filter
14. washwashed twice with 50 ml of anhydrous ether
15. customdried at 40° C/125 mm