반응 #457306

ord-98ea8cec25a647919a536e0861275368

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The precipitated product was filtered off
  2. 2
    workup.ADDITIONmixed with methylene chloride (500 ml)
  3. 3
    세척washed with 5% NaHCO3 solution (500 ml)
  4. 4
    농축The organic phase was concentrated by evaporation

실험 절차

Chlorine gas (17.5 g/0.25 mole) was passed at 0 to 50C into a suspension of 2,2'-dithiobisbenzthiazole (83 g/0.25 mole) in chlorobenzene (600 ml). Mercaptoethanol (39 g/0.5 mole) was then added drop-wise to this solution, followed by stirring for 7 hours at room temperature. The precipitated product was filtered off, mixed with methylene chloride (500 ml) and washed with 5% NaHCO3 solution (500 ml). The organic phase was concentrated by evaporation. A yellowish-brown oil (102 g) was obtained, which crystallised after a short time. m.pt.: 65 to 68° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06140427uspto-grants-2000_10