反应详情

温度

0 °C

A mixture of {5-[2-(1-cyano-cyclobutyl)-pyridin-4-yl]-4-methyl-thiazol-2-yl}-carbamic acid tert-butyl ester (Step 19.2) (640 mg, 1.73 mmol) and concentrated sulfuric acid is stirred for 40 min at 0° C., allowed to warm to rt, stirred for 1 h, quenched by addition of a saturated solution of NaHCO3 (50 mL) and extracted with DCM (3×75 mL). The organic phase is washed with a saturated solution of NaHCO3 (2×50 mL), dried (Na2SO4), filtered and concentrated. The residue is purified by silica gel column chromatography (DCM/MeOH/NH3aq, 99:0:1→93:6:1) to afford 35 mg of the title compound as a yellow solid: ESI-MS: 289.1 [M+H]+; TLC: Rf=0.32 (DCM/MeOH, 9:1).

1. temperatureto warm to rt
2. stirringstirred for 1 h
3. customquenched by addition of a saturated solution of NaHCO3 (50 mL)
4. extractionextracted with DCM (3×75 mL)
5. washThe organic phase is washed with a saturated solution of NaHCO3 (2×50 mL)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue is purified by silica gel column chromatography (DCM/MeOH/NH3aq, 99:0:1→93:6:1)