Potassium Phosphate, Tribasic → 6-(4-(3-hydroxypropyl)-3-(trifluoromethyl)phenyl)-1-methyl-1H-imidazo[4,5-c]pyridine-4-carbonitrile

温度

110 °C

6-Chloro-1-methyl-1H-imidazo[4,5-c]pyridine-4-carbonitrile (1.29 g), 3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trifluoromethyl)phenyl)propan-1-ol (2.432 g), tris(dibenzylideneacetone)dipalladium (0.307 g), tricyclohexylphosphine (0.225 g) and potassium phosphate (2.417 g) were suspended in dioxane (20 ml) and water (8 ml). The reaction mixture was placed under a nitrogen atmosphere and heated to reflux (110° C.) for 1.5 hours. The mixture was allowed to cool to room temperature then diluted with EtOAc (500 mL), filtered through celite and washed with water (200 mL). Organic layer was dried over sodium sulphate and solvent was evaporated under reduced pressure. The solid residue was washed with ether to afford 6-[4-(3-hydroxypropyl)-3-(trifluoromethyl)-phenyl]-1-methyl-1H-imidazo[4,5-c]pyridine-4-carbonitrile (1.5 g).

1. temperatureheated
2. temperatureto cool to room temperature
3. filtrationfiltered through celite
4. washwashed with water (200 mL)
5. dry with materialOrganic layer was dried over sodium sulphate and solvent
6. customwas evaporated under reduced pressure
7. washThe solid residue was washed with ether

ORDレコード

ord-f8f587fd0851489d88f52cf490b91096

出典データセット

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07932251B2