反应详情

A 0° C. mixture of Example A5 (1 g, 4.51 mmol) and pyridine (1.1 mL, 13.6 mmol) in DCM (25 mL) was treated with a solution of Example B2 (1.680 g, 7.22 mmol) in DCM (8 mL), warmed to RT and stirred 45 min. The mixture was concentrated to dryness, the residue treated with DCM and Et2O, sonicated and the resulting solid collected via filtration. The solid was dissolved in DCM, washed with water, the aqueous layer back-extracted with DCM (3×) and the combined organics were dried over Na2SO4 and concentrated to dryness to afford N-(5-((2-chloropyridin-4-yl)oxy)pyridin-2-yl)-2-oxo-3-(tetrahydro-2H-pyran-4-yl)imidazolidine-1-carboxamide (2.24 g, 119%) which was used without further purification. MS (ESI) m/z: 418.1 (M+H+).

1. concentrationThe mixture was concentrated to dryness
2. additionthe residue treated with DCM and Et2O
3. customsonicated
4. filtrationthe resulting solid collected via filtration
5. dissolutionThe solid was dissolved in DCM
6. washwashed with water
7. extractionthe aqueous layer back-extracted with DCM (3×)
8. dry with materialthe combined organics were dried over Na2SO4
9. concentrationconcentrated to dryness