反应详情

温度

126 °C

1-(2-Methanesulfinyl-pyrimidin-4-yl)-4-(3-methanesulfonyl-propoxy)-1H-indole (538 mg, 1.4 mmol), 4-(2-hydroxyprop-2-yl)-cyclohexylammonium acetate (400 mg, 2 mmol), and DIEA (0.8 mL, 5 mmol) were combined in NMP (10 mL) and heated to 126° C. in a sealed tube for 4 h, cooled, and partitioned between water and EtOAc. The organic layer was separated and washed twice with water, dried over sodium sulfate, filtered and purified by flash chromatography (SiO2) with 3:97 MeOH/DCM, and recrystallized from MeOH/DCM, triturated with EtOAc and solvent evaporated to yield 2-(4-{4-[4-(3-methanesulfonyl-propoxy)-indol-1-yl]-pyrimidin-2-ylamino}-cyclohexyl)-propan-2-ol (Compound 166, 391 mg, 59%) as a white powder.

1. temperaturecooled
2. custompartitioned between water and EtOAc
3. customThe organic layer was separated
4. washwashed twice with water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. custompurified by flash chromatography (SiO2) with 3:97 MeOH/DCM
8. customrecrystallized from MeOH/DCM
9. customtriturated with EtOAc and solvent
10. customevaporated