Phosphoric Acid → HCID 57558445, Verbindung

Temperatur

-75 °C

To a 100 mL round bottom flask is added 2′,6′ dihydroxypropiophenone (25 g, 0.15 mol) and to it is then added dichloromethane (50 mL). This is then cooled to −75° C. and then 2.6 mL of H3PO4 is added to it followed by 6.22 mL of boron trifluoride etherate and then isobutylene (125 mL). The reaction is then stirred at −75° C. for 1.5 hrs and then at room temperature overnight. The reaction mixture is then poured into a 2N ammonium hydroxide solution (200 mL) and extracted with dichloromethane. The organic layer is then washed with water and then with brine and dried over sodium sulfate and filtered. The crude residue obtained after concentration of the filtrate is purified by flash chromatography using silica gel (ethyl acetate:hexanes) to afford the above product.

1. customat room temperature
2. customovernight
3. extractionextracted with dichloromethane
4. washThe organic layer is then washed with water
5. dry with materialwith brine and dried over sodium sulfate
6. filtrationfiltered

ORD-Eintrag

ord-ba5e83784a10452dbcdb268072805979

Quelldatensatz

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08263042B2