反应详情

To a solution of 2.73 g (0.01 mol) of 2-imino-3-phenylmethylthiazolidine hydrobromide in 10 ml of water 1.36 g of anhydrous sodium acetate and 0.62 ml of glacial acetic acid are added, then 0.75 g of sodium nitrite dissolved in 3 ml of water is dropped to the above mixture at 5° C. under stirring, then the mixture is stirred at 5° C. for additional 3 hours. After standing in a refrigerator overnight, the solution is stirred at room temperature for 3 hours. After rubbing, a precipitate appears which is filtered off, washed with water, dried and then refluxed with five volumes of n-butanol for 2 hours. After evaporating the solvent, the residue is thoroughly rubbed with diisopropyl ether and the product is filtered off. Thus, 0,81 g (42.3%) of the title product is obtained, m.p.: 49°-50° C.

1. additionis dropped to the above mixture at 5° C.
2. stirringthe mixture is stirred at 5° C. for additional 3 hours
3. customAfter standing in a refrigerator overnight
4. stirringthe solution is stirred at room temperature for 3 hours
5. filtrationis filtered off
6. washwashed with water
7. customdried
8. temperaturerefluxed with five volumes of n-butanol for 2 hours
9. customAfter evaporating the solvent
10. filtrationthe product is filtered off