反应详情

温度

120 °C

trans-4-Aminocyclohexanol (870 mg, 8 mmol) was added to 1-(2-methanesulfonyl-pyrimidin-4-yl)-3-methoxy-1H-indazole (440 mg, 1 mmol) in NMP (15 mL), and the resulting mixture heated to 120° C. for 3 h. The reaction mixture was cooled and partitioned between EtOAc and water. The organic layer was separated, washed with water, dried over Na2SO4, filtered, and concentrated under reduced pressure to give a crude yellow solid. This crude material was purified by flash chromatography (MeOH/DCM, 5:95) and recrystallized from DCM/hexanes to give trans-4-[4-(3-methoxy-indazol-1-yl)-pyrimidin-2-ylamino]-cyclohexanol (181 mg (37% yield) as a white solid. MS=340 [M+H]+; MP=202.3-205.1° C.

1. temperatureThe reaction mixture was cooled
2. custompartitioned between EtOAc and water
3. customThe organic layer was separated
4. washwashed with water
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customto give a crude yellow solid
9. customThis crude material was purified by flash chromatography (MeOH/DCM, 5:95)
10. customrecrystallized from DCM/hexanes