反应详情

To a solution of 50.0 g of 2-methylamino-5-(β-chloro-α,α-dimethylethyl)-1,3,4-thiadiazole in 300 ml of pyridine was added 46.0 g of dimethyl carbamyl chloride and the reaction heated at reflux temperature for 16 hrs. After cooling, the pyridine was removed on the rotary evaporator and water added to the residue. The reaction was extracted with ether which was shaken with water, saturated sodium chloride and dried over Na2SO4. The solvent was removed at reduced pressure giving 60 g of a viscous oil. Crystallization was effected using a mixture of ether-petroleum ether; wt. 34.5 g (52%), m.p. 80°-82°. Recrystallization from ether-petroleum ether gave the analytical sample, m.p. 82°-83°.

1. temperaturethe reaction heated
2. temperatureat reflux temperature for 16 hrs
3. temperatureAfter cooling
4. customthe pyridine was removed on the rotary evaporator and water
5. additionadded to the residue
6. extractionThe reaction was extracted with ether which
7. dry with materialdried over Na2SO4
8. customThe solvent was removed at reduced pressure