反应详情

4-Chloro-6-(2-chloro-4-pyridyl)-2-methylthio-5-(3-(trifluoromethyl)-phenyl)pyrimidine (0.873 g, 2.1 mmol) and 16.5 ml of NH2NH2—H2O in 90 ml EtOH in a 150-ml r.b.flask with a stir bar was stirred at 70° C. The reaction was cooled to room temperature. The solvents were evaporated in vacuo. The residue was dried by addition and removal of toluene in vacuo and further dried under vacuum at 50° C. overnight. The resulting light yellow solid was mixed with 40 ml of DCM, 20 ml of CH(OCH3)3, and 10 ml of TFA in a 150-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 by sat'd NaHCO3. The DCM layer was washed with brine (3×20 ml) and dried over Na2SO4. After removal of the DCM in vacuo, crude product (MS m/z 421.8 (M+H)+) was obtained as a dark brown oil, which was used directly in the next step.

1. customThe solvents were evaporated in vacuo
2. dry with materialThe residue was dried by addition and removal of toluene in vacuo
3. customfurther dried under vacuum at 50° C. overnight
4. additionThe resulting light yellow solid was mixed with 40 ml of DCM, 20 ml of CH(OCH3)3, and 10 ml of TFA in a 150-ml r.b.flask with a stir bar
5. washThe DCM layer was washed with brine (3×20 ml)
6. dry with materialdried over Na2SO4
7. customAfter removal of the DCM in vacuo
8. customcrude product (MS m/z 421.8 (M+H)+) was obtained as a dark brown oil, which