反应详情

A solution of 0.28 g of 4-chloro-5-(4-fluoro phenyl)-2-methylthio-6-(4-pyridyl)pyrimidine (0.85 mmol) and 3 ml of NH2NH2—H2O in 20 ml EtOH in a 50-ml r.b.flask with a stir bar was stirred at 70° C. The solvents were evaporated and the residue was mixed with toluene. The residue was dried by removal water with toluene and further dried under vacuum at 50° C. overnight. The resulting light yellow solid was mixed with 40 ml of DCM, 4 ml of CH(OCH3)3, and 2 ml of TFA in a 100-ml r.b.flask with a stir bar. The reaction solution was stirred at RT overnight. The acidic reaction solution was neutralized to pH 8 with sat'd NaHCO3. The DCM layer was washed with brine (10 ml) and dried over Na2SO4. After removal of the DCM in vacuo, 8-(4-fluorophenyl)-5-methylthio-7-(4-pyridyl)-1,2,4-triazolo[4,3-c]pyrimidine was obtained as yellow solid; MS m/z (M+H)+ 338.1; C17H12FN5S requir. 337.3.

1. customThe solvents were evaporated
2. additionthe residue was mixed with toluene
3. dry with materialThe residue was dried by removal water with toluene
4. customfurther dried under vacuum at 50° C. overnight
5. additionThe resulting light yellow solid was mixed with 40 ml of DCM, 4 ml of CH(OCH3)3, and 2 ml of TFA in a 100-ml r.b.flask with a stir bar
6. washThe DCM layer was washed with brine (10 ml)
7. dry with materialdried over Na2SO4
8. customAfter removal of the DCM in vacuo