反应详情

温度

150 °C

7-Methoxy-2-[1-methyl-4-phenyl-2-(3-thienyl)-1H-imidazol-5-yl][1,3]thiazolo[5,4-d]pyrimidine (Intermediate 44) (26 mg) was dissolved in 0.5M NH3 in 1,4-dioxane (3 mL)/concentrated aqueous NH3 (0.6 mL), sealed and heated under microwave conditions (CEM explorer, 150° C., 150 W) for 1 hour. After which the reaction mixture was concentrated in vacuo, dissolved in EtOAc (20 mL), washed: with 2M NaOH (2×10 mL) then brine (1×15 mL), dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluting with 4% MeOH/DCM gave the title compound as an off-white solid (17 mg, 68%);

1. customsealed
2. concentrationAfter which the reaction mixture was concentrated in vacuo
3. dissolutiondissolved in EtOAc (20 mL)
4. washwashed
5. dry with materialwith 2M NaOH (2×10 mL) then brine (1×15 mL), dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification by flash chromatography on silica eluting with 4% MeOH/DCM