Reaktion #1981896

ord-0f2d04f8425f410aaa6f0dee9c379248

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting reaction mixture
  2. 2
    Temperaturwas heated
  3. 3
    Temperaturto reflux for 3 hr
  4. 4
    EinengenThe reaction was concentrated
  5. 5
    Sonstigechromatographed on silica gel eluting with a gradient solvent mixture of AcOEt & dichloromethane

Vorschrift

To a 37.5 mL THF solution of tert-butyl[2-(2-acetylhydrazino)-2-oxoethyl]carbamate (496 mg, 2.15 mmol) was added Lawesson's reagent (900 mg, 2.23 mmol). The resulting reaction mixture was heated to reflux for 3 hr. The reaction was concentrated and chromatographed on silica gel eluting with a gradient solvent mixture of AcOEt & dichloromethane to give the title compound as white crystalline solid (391 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08513289B2uspto-grants-2013_08