Reaktion #340244

ord-617be5223ca14dafa4ffe2639fa7320f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    EinengenThe reaction mixture was concentrated in vacuo and to the residue
  3. 3
    workup.ADDITIONwas added diethyl ether-hexane (1/1)
  4. 4
    workup.ADDITIONThereto was added 4M HCl-ethyl acetate (1.05 mL)
  5. 5
    Filtrationthe precipitates were collected by filtration
  6. 6
    Sonstigedried

Vorschrift

A solution of 1-aminocyclohexanecarboxylic acid (600 mg) in tetrahydrofuran-methanol was stirred under ice-cooling. Thereto was added dropwise a (trimethylsilyl) diazomethane solution (4.2 mL) and the mixture was stirred overnight. The reaction mixture was concentrated in vacuo and to the residue was added diethyl ether-hexane (1/1). Thereto was added 4M HCl-ethyl acetate (1.05 mL) and the precipitates were collected by filtration and dried to give 1-amino-1-methoxy-carbonylcyclohexane (423 mg, yield: 52%) as a white powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07872006B2uspto-grants-2011_01