Isopropanol → (R)-2-(3,4-Difluorophenyl)-4-[3-(tert-butyldimethylsiloxy)-1-butoxy]-5-[4-(methylthio)phenyl]-3(2H)-pyridazinone

Temperatur

70 °C

Under a nitrogen atmosphere, a mixture of the product from Example 545C (0.98 g, 2 mmol), 4-(methylthio)benzeneboronic acid (0.4 g, 2.4 mmol), K3PO4 (1.2 g, 6 mmol), PdCl2(PPh3)2 (28 mg, 0.04 mmol), isopropanol (9 mL), and water (1 mL) was stirred at 70° C. for 4 hours. The reaction mixture was then cooled to room temperature, water (30 mL) was added and stirring was continued for 2 hours. The crude black precipitate was collected by filtration then Washed with water (10 mL) and hexane (10 mL). This title intermediate was used without further purification in the following oxidation/deprotection step.

1. temperatureThe reaction mixture was then cooled to room temperature
2. stirringstirring
3. waitwas continued for 2 hours
4. filtrationThe crude black precipitate was collected by filtration
5. washthen Washed with water (10 mL) and hexane (10 mL)
6. customThis title intermediate was used without further purification in the following oxidation/deprotection step

ORD-Eintrag

ord-dab3acf4c7d942c1abaeef394f09eff1

Quelldatensatz

uspto-grants-2006_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07001895B2