Reaktion #61386

ord-b07f7d877af1452ca4c32d8926e06992

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was filtered through Celite
  2. 2
    workup.ADDITIONThe filtrate was diluted with EtOAc
  3. 3
    Waschenwashed with water
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Einengenconcentrated under vacuum

Vorschrift

A mixture of 1-[3-(2-chloro-1-chloromethyl-ethoxy)-2-nitro-phenylmethanesulfonyl]-naphthalene (3) (2.4 g, 5.3 mmoles) and 10% Pd/C in a 1:1 mixture of THF and methanol was hydrogenated on a Parr hydrogenator at 40 lb/in2 for 20 hours. The mixture was filtered through Celite. The filtrate was diluted with EtOAc, washed with water, dried over Na2SO4, and concentrated under vacuum to afford the title compound as an off white solid (2.02 g, 4.77 mmoles), identified by HNMR analysis.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429582B2uspto-grants-2008_09