反应详情

温度

120 °C

trans-4-Aminocyclohexanol (0.45 g, 4 mmol) was added to 3-(2-chloropyrimidin-4-yl)-1-methyl-1H-indole (0.23 g, 1 mmol) in NMP (8 mL), and the resulting mixture heated to 120° C. for 3 h. A second aliquot of trans-4-aminocyclohexanol (0.16 g, 1 mmol) was added, and the resulting mixture was heated to 130° C. The reaction mixture was cooled and partitioned between water and EtOAc, the organic layer separated, washed twice with water, dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude residue was recrystallized from DCM/EtOAc/hexanes to give trans-4-[4-(1-methyl-1H-indol-3-yl)-pyrimidin-2-ylamino]-cyclo-hexanol (148 mg, 46% yield) as a light-yellow solid. MS=323 [M+H]+; MP=194.5-195.3° C.

1. temperaturethe resulting mixture was heated to 130° C
2. temperatureThe reaction mixture was cooled
3. custompartitioned between water and EtOAc
4. customthe organic layer separated
5. washwashed twice with water
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe crude residue was recrystallized from DCM/EtOAc/hexanes