反应详情

温度

40 °C

To a solution of the above 5-fluoro-2,4-dichloropyridine (67 mg, 0.4 mol) in EtOH (2 mL) were added tert-butyl trans-4-aminomethylcyclohexylcarbamate (100 mg, 0.44 mmol) and DIPEA (77 μL, 0.44 mmol). The reaction mixture was heated at 40° C. for 1 h. The mixture was concentrated in vacuo and the resulting residue was dissolved in EtOAc and washed with brine. The aqueous layer was re-extracted with EtOAc (×2). The combined organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo to yield 127 mg (89%) of {4-[(2-chloro-5-fluoro-pyrimidin-4-ylamino)-methyl]-cyclohexyl}-carbamic acid tert-butyl ester.

1. concentrationThe mixture was concentrated in vacuo
2. dissolutionthe resulting residue was dissolved in EtOAc
3. washwashed with brine
4. extractionThe aqueous layer was re-extracted with EtOAc (×2)
5. dry with materialThe combined organic phase was dried over anhydrous Na2SO4
6. concentrationconcentrated in vacuo