Water → 2-[3,4-Bis(difluoromethoxy)phenyl]ethanol

Temperatur

60 °C

To a solution of 1,2-bis(difluoromethoxy)-4-vinylbenzene (10 g, 0.0431 mol; see step (iii) above) in 25 mL of THF was added, dropwise, borane-methyl sulfide complex (10 mmol; 10 mL of a 1 M solution in THF). The resulting mixture was stirred at 60° C. for 1 h, before being cooled to RT. Excess borane was decomposed by adding few drops of water and the resultant mixture refluxed for 1 h with 2 M NaOH (100 mL) 50% H2O2 (87 mL). The mixture was then extracted with dichloromethane, washed with water and then brine, and dried over sodium sulfate. Solvent evaporation under reduced pressure gave the sub-title compound as a pale yellow liquid. Yield: 6 g.

1. temperaturebefore being cooled to RT
2. extractionThe mixture was then extracted with dichloromethane
3. washwashed with water
4. dry with materialbrine, and dried over sodium sulfate
5. customSolvent evaporation under reduced pressure

ORD-Eintrag

ord-dd9b3e48c6614fb7a1406b10408b226b

Quelldatensatz

uspto-grants-2010_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07648985B2