Cesium carbonate → 6-(3-(6-amino-5-(trifluoromethyl)pyridin-3-yl)-1-isopropyl-1H-pyrazol-5-yl)bicyclo[3.1.0]hexan-2-ol

温度

110 °C

A solution of (±)-6-(3-iodo-1-isopropyl-1H-pyrazol-5-yl)bicyclo[3.1.0]hexan-2-ol (30 mg, 90.3 μmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-(trifluoromethyl)pyridin-2-amine (39 mg, 0.14 mmol), 1,1′-bis(diphenylphosphino)ferrocene-palladium(II) dichloride (6 mg, 0.009 mmol) and cesium carbonate (59 mg, 0.18 mmol) in 1,4-dioxane (0.5 mL) and water (0.1 mL) was purged with nitrogen. The reaction mixture was heated to 110° C. by microwave irradiation for 20 min. The mixture was concentrated, and the resulting residue was diluted with ethyl acetate (2 mL), and the solution was filtered. The filtrate was concentrated. Purification by preparation HPLC followed by chiral SFC separation afforded the title compounds:

1. concentrationThe mixture was concentrated
2. additionthe resulting residue was diluted with ethyl acetate (2 mL)
3. filtrationthe solution was filtered
4. concentrationThe filtrate was concentrated
5. customPurification
6. customby preparation HPLC
7. customfollowed by chiral SFC separation

ORDレコード

ord-b1a57cdd1fa34c70ab3e971a8262add2

出典データセット

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09365583B2