Water → HCID 5276006, Verbindung

Temperatur

90 °C

In a flame dried vial with a Teflon lined screw cap, a solution of Compound 365b (100 mg, 0.175 mmol), 4-amidophenylboronic acid (31 mg, 0.2625 mmol), and Palladium Tetrakis (20 mg, 0.0175 mmol) in toluene (6.5 mL), methanol (1.6 mL), and saturated sodium bicarbonate in water (800 ul) was degassed, flushed with argon, and sealed. The reaction was stirred for 16 hours at 90° C. The vial was then cooled to room temperature and 10% w/v KOH in methanol (2 mL, 3.5 mmol) was added. The reaction was resealed and stirred at 70° C. for 1 hour. The completed reaction was then evaporated to dryness, purified via HPLC, and converted to the HCl salt using the standard procedure (as described for Compound 516) to produce the title compound.

1. dry with materialIn a flame dried vial with a Teflon lined screw
2. customcap
3. customflushed with argon
4. customsealed
5. temperatureThe vial was then cooled to room temperature
6. additionwas added
7. stirringstirred at 70° C. for 1 hour
8. customThe completed reaction
9. customwas then evaporated to dryness
10. custompurified via HPLC

ORD-Eintrag

ord-147c10f1b8ef4deabab477614815e219

Quelldatensatz

uspto-grants-2009_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07511145B2