Lawesson's reagent → HCID 86650591, Verbindung

Temperatur

80 °C

To a solution (30 mL) of the compound (3.7 g, 14 mmol) obtained in Example 77a in tetrahydrofuran was added 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (5.5 g, 14 mmol), and the mixture was stirred at 80° C. for 5 hr. Saturated aqueous sodium hydrogen carbonate was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting crude title compound was recrystallized (hexane-ethyl acetate) to give the title compound (3.2 g, 83%) as pale-yellow crystals.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe obtained organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customThe resulting crude title compound was recrystallized (hexane-ethyl acetate)

ORD-Eintrag

ord-2e85c61dec094b3e86af6cdf10b804f9

Quelldatensatz

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08461348B2