反应详情

A solution of 57.6 g (0.338 mol) of 3-tert.butyl-5-methylthio-4H-1,2,4-triazole and 38g (0.355 mol) of dimethylcarbamyl chloride in 300 ml of pyridine was maintained at reflux temperature for 16 hrs. After the pyridine was removed at reduced pressure on the rotary evaporator, water was added followed by chloroform. The organic layer was washed with successive portions of dilute hydrochloric acid, water and brine then dried over Na2SO4. The solvent was removed in vacuo to give 75 g, nD26 1.5165 of an oil. Spectral properties agree with the structure

1. temperatureat reflux temperature for 16 hrs
2. customAfter the pyridine was removed at reduced pressure on the rotary evaporator, water
3. additionwas added
4. washThe organic layer was washed with successive portions of dilute hydrochloric acid, water and brine
5. dry with materialthen dried over Na2SO4
6. customThe solvent was removed in vacuo
7. customto give 75 g