反应详情

Sodium hydride (81.8 mg, 2.0 mmol) was added to a solution of cis-3-(benzothiazol-2-ylamino)-cyclobutanol (150 mg, 0.68 mmol) in DMF (3 mL) under argon and the mixture was stirred for 1 h at RT. Then 2,5-difluoro-3-(tetrahydro-pyran-4-yl)-pyridine, as prepared in Example 4, steps 1-4, (162 mg, 0.82 mmol) was added and the resulting mixture was heated to 100° C. for 2 h. It was cooled to RT and EtOAc and saturated NH4Cl were added. The organic layer was separated, washed with water (2×25 mL), brine (25 mL), dried over MgSO4, filtered and concentrated in vacuo to give oil, which was purified by prep-HPLC to give product (20 mg). [M+1] 400. IC50 (uM) 0.0002.

1. additionwas added
2. temperaturethe resulting mixture was heated to 100° C. for 2 h
3. temperatureIt was cooled to RT
4. customThe organic layer was separated
5. washwashed with water (2×25 mL), brine (25 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customto give oil, which
10. customwas purified by prep-HPLC