反应详情

温度

90 °C

To a solution of 2-(methylthio)-5-(prop-1-yn-1yl)pyrimidine-4-carboxamide (Preparation 50, 270 mg, 1.303 mmol) in toluene (30 mL) was added pTSA (50 mg, 0.261 mmol). The reaction mixture was heated to 90° C. for 18 hours. The reaction mixture was concentrated in vacuo. The residue was dissolved in NH3 in MeOH (7M, 10 mL) and heated to 80° C. for 18 hours. The reaction mixture was concentrated in vacuo. The residue was purified by column chromatography eluting with 0-5% MeOH in DCM to give the title compound (150 mg, 56%).

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved in NH3 in MeOH (7M, 10 mL)
3. temperatureheated to 80° C. for 18 hours
4. concentrationThe reaction mixture was concentrated in vacuo
5. customThe residue was purified by column chromatography
6. washeluting with 0-5% MeOH in DCM