反应详情

1-(2-Methanesulfinyl-pyrimidin-4-yl)-4-(3-methanesulfonyl-propoxy)-1H-indole (5.0 g, 13 mmol) and (4-amino-cyclohexyl)-methanol hydrochloride (2.46 g, 19 mmol) were heated at reflux in EtOH (100 mL) under N2 for 16 h. The reaction mixture was then cooled, the suspension filtered, the filtrate volume reduced by half, diluted with EtOAc and washed with water, dried over sodium sulfate, filtered and concentrated until precipitate formed. This suspension was filtered, and the filtrate concentrated again until precipitation, and the suspension filtered, and both precipitates were combined and solvent removed in vacuo to yield (4-{4-[4-(3-methanesulfonyl-propoxy)-indol-1-yl]-pyrimidin-2-ylamino}-cyclohexyl)-methanol (Compound 214, 2.93 g), as a light yellow powder.

1. temperatureThe reaction mixture was then cooled
2. filtrationthe suspension filtered
3. additiondiluted with EtOAc
4. washwashed with water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated until precipitate
8. customformed
9. filtrationThis suspension was filtered
10. concentrationthe filtrate concentrated again until precipitation
11. filtrationthe suspension filtered
12. customsolvent removed in vacuo