Reaktion #10202

ord-032980fbd7fc499094c1d87313b64b51

Reaktionsgleichung

O=C(N1CC2CC(C1)c1ccccc12)C(F)(F)F
1-(10-Aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone
O=S(=O)(O)Cl
chlorosulfonic acid
O=C(N1CC2CC(C1)c1cc(S(=O)(=O)Cl)ccc12)C(F)(F)F
oil
Ausbeute 87.0%
O=C(N1CC2CC(C1)c1cc(S(=O)(=O)Cl)ccc12)C(F)(F)F
10-Trifluoroacetyl-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-triene-4-sulfonyl chloride
Ausbeute 87.0%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was quenched with ice
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    Trocknendried (Na2SO4)
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated

Vorschrift

1-(10-Aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone mg, 2.1 mmol) was added to chlorosulfonic acid (2 mL, 30 mmol) and stirred for 5 minutes. The mixture was quenched with ice, extracted with ethyl acetate, dried (Na2SO4), filtered and concentrated to provide an oil (640 mg, 87%). (TLC 30% ethyl acetate/hexanes Rf 0.15).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091372B2uspto-grants-2006_08