反应详情

温度

0 °C

Dissolve 5-[4-(azetidin-3-yloxy)-3-methoxy-phenyl]-2-(4-chloro-phenyl)-5H-thiazolo[5,4-c]pyridin-4-one (75 mg, 0.171 mmol) and triethylamine (52.5 μL, 0.376 mmol) in dry CH2Cl2 (700 μL). Chill to 0° C. and add acetylchloride (13.4 μL, 0.188 mmol). Allow to warm to room temperature overnight. Add 1 N HCl solution and extract with CH2Cl2 (3×5 mL). Combine the organic portions and wash with water (2×5 mL). Dry the organic layer with Na2SO4, filter, and concentrate in vacuo. Purify the resulting residue on HPLC with 5 μm 30×75 mm XBridge C18 column; eluent: 34% water (with 10 mM NH4HCO3 added to pH=10/acetonitrile (isocratic) to give 39 mg, (48%). ES/MS m/z (35Cl) 481.8 [M+1]+.

1. temperatureAllow to warm to room temperature overnight
2. extractionextract with CH2Cl2 (3×5 mL)
3. washCombine the organic portions and wash with water (2×5 mL)
4. dry with materialDry the organic layer with Na2SO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customPurify the resulting residue on HPLC with 5 μm 30×75 mm XBridge C18 column
8. additioneluent: 34% water (with 10 mM NH4HCO3 added to pH=10/acetonitrile (isocratic)
9. customto give 39 mg, (48%)