反应详情

To a stirred solution of 2-methylpyrimidine-5-carboxylic acid (23 mg, 0.17 mmol) in DCM (3 ml) was added HOBt (23 mg, 0.17 mmol) and HBTU (64 mg, 0.17 mmol). After 3 hours, a solution of 1-(Azetidin-3-ylcarbonyl)-4-cyclobutyl-1,4-diazepane (48 mg, 0.17 mmol), in DCM (1 ml) was added and the yellow suspension gradually dissolved to give a yellow solution. The reaction mixture was quenched with saturated NaHCO3 (1 ml) and the aqueous layer extracted with DCM (3×5 ml). The combined organic layers were dried (MgSO4), filtered and concentrated at reduced pressure. Purification by silica FCC (eluting with 99:1 to 95:5 gradient of DCM/2M NH3 in MeOH) gave the title compound (17.4 mg, 29% yield) as pale yellow oil.

1. dissolutionthe yellow suspension gradually dissolved
2. customto give a yellow solution
3. customThe reaction mixture was quenched with saturated NaHCO3 (1 ml)
4. extractionthe aqueous layer extracted with DCM (3×5 ml)
5. dry with materialThe combined organic layers were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated at reduced pressure
8. customPurification
9. washby silica FCC (eluting with 99:1 to 95:5 gradient of DCM/2M NH3 in MeOH)