反应详情

2-Amino-5-methyl-1,3,4-thiadiazole (23 g, 0.2 mole) and benzaldehyde (29.6 ml, 0.3 mole) were refluxed together in ethanol (200 ml) for 11/2 hours. The solution was cooled to room temperature and sodium borohydride (11.35 g, 0.3 mole) added over 5 to 10 minutes. The mixture was refluxed for 4 hours, treated with further sodium borohydride (5 g) and refluxed overnight. The ethanol was evaporated off, the residue treated with water and extracted with ether. The ether extract was dried over sodium sulphate, filtered and evaporated to leave an oil which solidified. This solid was triturated with ether, filtered, washed with light petroleum (b.p. 40°-60° C.) and again triturated with ether and filtered to give N-(5-methyl-1,3,4-thiadiazol-2-yl)-benzylamine (30.95 g), which on recrystallisation from ether had m.p. 140° C.

1. temperatureThe mixture was refluxed for 4 hours
2. temperaturerefluxed overnight
3. customThe ethanol was evaporated off
4. additionthe residue treated with water
5. extractionextracted with ether
6. extractionThe ether extract
7. dry with materialwas dried over sodium sulphate
8. filtrationfiltered
9. customevaporated
10. customto leave an oil which
11. customThis solid was triturated with ether
12. filtrationfiltered
13. washwashed with light petroleum (b.p. 40°-60° C.)
14. customagain triturated with ether
15. filtrationfiltered