Triethylamine → (R)-N-(4-(4-((1-(methylsulfonyl)pyrrolidin-3-yl)oxy)phenyl)pyrazolo[1,5-a]pyridin-2-yl)cyclopropanecarboxamide

温度

0 °C

(R)—N-(4-(4-(pyrrolidin-3-yloxy)phenyl)pyrazolo[1,5-a]pyridin-2-yl)cyclopropanecarboxamide (340 mg, 0.94 mmol) and triethylamine (0.16 ml, 1.13 mmol) were suspended in DCM (10 ml) and stirred at 0° C. under N2. Methane sulfonylchloride (77 μL, 0.99 mmol) was added slowly and the resulting solution was allowed to warm to room temperature over 4 h. The reaction mixture was washed with sat. NaHCO3 solution (aq.) and the aqueous phase extracted with DCM. The combined organics were dried (MgSO4), filtered, concentrated in vacuo and purified by preparative HPLC to give (R)—N-(4-(4-((1-(methylsulfonyl)pyrrolidin-3-yl)oxy)phenyl)pyrazolo[1,5-a]pyridin-2-yl)cyclopropanecarboxamide. (126 mg, 30% yield).

1. temperatureto warm to room temperature over 4 h
2. washThe reaction mixture was washed with sat. NaHCO3 solution (aq.)
3. extractionthe aqueous phase extracted with DCM
4. dry with materialThe combined organics were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. custompurified by preparative HPLC

ORDレコード

ord-497bfc48b1254cfe8b72962b5ff305aa

出典データセット

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08975406B2