Dichloromethane → [6-Amino-5-(trifluoromethyl)pyridin-3-yl]boronic acid

5-bromo-3-(trifluoromethyl)pyridin-2-amine (9.85 mmol, commercially available), Bis(pinacolato)diboron (11.82 mmol), potassium acetate (1.4 g) and (1,1-bis(diphenylphosphino)ferrocene)-dichloropalladium (II) complex with DCM (200 mg, commercially available) was dissolved in dioxane (75 mL) under argon atmosphere. The reaction mixture was refluxed for 8 h. The reaction mixture was cooled, diluted with ethyl acetate (75 mL) and filtered. The filtrate was concentrated. The crude product was purified over silica gel using 0-10% ethyl acetate in petroleum ether to obtain the titled boronic acid derivative.

1. temperatureThe reaction mixture was refluxed for 8 h
2. temperatureThe reaction mixture was cooled
3. filtrationfiltered
4. concentrationThe filtrate was concentrated
5. customThe crude product was purified over silica gel using 0-10% ethyl acetate in petroleum ether

ORDレコード

ord-e4a56016496947f6bacc45c5abcb4431

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09062046B2