Reaktion #1857926

ord-e79538a208514dc2bab55a69f72a986c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was filtered through Celite
  2. 2
    Einengenconcentrated in vacuo
  3. 3
    Sonstigeto give 20 g of a crude liquid, which
  4. 4
    workup.DISTILLATIONwas distilled under vacuum (<1 mbar, 100-125° C.)

Vorschrift

To a solution of 2-((2-methyl-2-nitropropyl)amino)ethanol (20.4 g, 126 mmol) in methanol (120 ml) was added a slurry of 50% Raney Nickel® in H2O (6 ml). The vessel was pressurized with H2 (450 psi) and the suspension stirred for 19 h. The mixture was filtered through Celite and concentrated in vacuo to give 20 g of a crude liquid, which was distilled under vacuum (<1 mbar, 100-125° C.) to give 13 g of a clear liquid, which was found to be partially purified and was used directly in the next step without purification. LRMS (ESI/APCI) m/z 133 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09248117B2uspto-grants-2016_02