Water → HCID 59227388, compound

Temperature

100 °C

To the mixture of sodium 2,6-dichlorobenzyloxymethyl trifluoroborate (41 mg, 0.15 mmol) synthesized in Example 10 and 1,4-dioxane (1.5 ml), water (0.15 ml), cesium carbonate (170 mg, 0.51 mmol), palladium(II) acetate (3.3 mg, 0.015 mmol), and 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (12 mg, 0.030 mmol) were added at room temperature, and the obtained reaction mixture was then stirred at 100° C. (an outer temperature) for 4 hours. The reaction mixture was cooled to room temperature, and then dichloromethane was added thereto. The organic layer was then separated and the solvents were evaporated under reduced pressure from the organic layer. The obtained residue was purified with silica gel column chromatography (hexane: diethyl ether=100:0→91:9→80:20), thereby obtaining the entitled compound (3.7 mg, 17%).

1. additionwere added at room temperature
2. customthe obtained reaction mixture
3. temperatureThe reaction mixture was cooled to room temperature
4. customThe organic layer was then separated
5. customthe solvents were evaporated under reduced pressure from the organic layer
6. customThe obtained residue was purified with silica gel column chromatography (hexane: diethyl ether=100:0→91:9→80:20)

ORD record

ord-418a97fd2bd54c0cb9cbe759bb704846

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08273885B2