反应详情

温度

22 °C

4-Amino-2-mercaptopyrimidine (0.40 g, 3.15 mmol) is slurried in ethanol (2 ml) and 3.25 M NaOH (2.0 ml, 6.5 mmol) is added. The solution is heated to reflux for 10 minutes and after cooling to 22° C., 2-picolyl chloride*HCl (0.49 g, 2.98 mmol) is added. The solution is heated to reflux for an additional 15 minutes. The solution is cooled and concentrated in vacuo. The residue is dissolved in 1 N HCl and diluted with ethyl acetate. The mixture is neutralized with NaOH to pH 8 and the aqueous layer is separated and washed twice with ethyl acetate. The combined organic layers are washed with saturated NaHCO3, saturated NaCl, dried with MgSO4 and concentrated in uacuo, mp 133-134° C.

1. temperatureThe solution is heated
2. temperatureto reflux for 10 minutes
3. temperatureThe solution is heated
4. temperatureto reflux for an additional 15 minutes
5. temperatureThe solution is cooled
6. concentrationconcentrated in vacuo
7. dissolutionThe residue is dissolved in 1 N HCl
8. additiondiluted with ethyl acetate
9. customthe aqueous layer is separated
10. washwashed twice with ethyl acetate
11. washThe combined organic layers are washed with saturated NaHCO3, saturated NaCl
12. dry with materialdried with MgSO4
13. concentrationconcentrated in uacuo, mp 133-134° C.