Sulfuric Acid → 4-Hydroxyphenylsulfur pentafluoride

Temperatur

0 °C

40.00 g of 4-pentafluorosulfanylaniline were suspended in 500 ml of a 35% aqueous H2SO4 solution and a solution of 13.85 g of NaNO2 in 30 ml of water was added dropwise at 0° C. over a period of 10 minutes. Subsequently, the mixture was stirred at 0° C. for 35 minutes, then a solution, at 0° C., of 171.10 g of Cu(NO3)2 in 200 ml of water was poured in and, directly thereafter, 26.11 g of Cu2O were added in portions. The mixture is stirred at RT for a further 2 hours, then extraction is effected 3 times with 200 ml each time of CH2Cl2. Drying was effected over MgSO4 and the solvent was removed under reduced pressure. 38.00 g of a pale yellow oil were obtained which was used further without purification.

1. additionwere added in portions
2. stirringThe mixture is stirred at RT for a further 2 hours
3. extractionextraction
4. customDrying
5. customthe solvent was removed under reduced pressure

ORD-Eintrag

ord-b0a05091a2ec430390a7f76578b9d27d

Quelldatensatz

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07932416B2