Reaktion #701545

ord-19ba23c697d24fa38c5f7227883ba5e1

Reaktionsgleichung

COc1ccccc1OCC(O)CN1CCC(=O)CC1
1-[2-hydroxy-3-(2-methoxyphenyloxy)-propyl]-piperidine-4-one
NCCNc1ccccc1
N-(2-aminoethyl)-aniline
[H][H]
hydrogen
COc1ccccc1OCC(O)CN1CCC(NCCNc2ccccc2)CC1
1-[2-hydroxy-3-(2-methoxyphenyloxy)-propyl]-4-(2-anilino-ethylamino)-piperidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe catalyst is thereafter removed by filtration
  2. 2
    Einengenthe filtrate is concentrated under reduced pressure
  3. 3
    SonstigeThe residue is freed from excess starting material in a bulb tube at 0.3 mm Hg and 120° C oven temperature

Vorschrift

A solution of 16.7 g of 1-[2-hydroxy-3-(2-methoxyphenyloxy)-propyl]-piperidine-4-one and 10.5 g of N-(2-aminoethyl)-aniline in 250 ml of methanol, with the addition of 1 g of a 5% platinum on charcoal catalyst is hydrogenated at room temperature and under normal pressure until 1 molar equivalent of hydrogen has been taken up. The catalyst is thereafter removed by filtration and the filtrate is concentrated under reduced pressure. The residue is freed from excess starting material in a bulb tube at 0.3 mm Hg and 120° C oven temperature to yield as distillation residue 1-[2-hydroxy-3-(2-methoxyphenyloxy)-propyl]-4-(2-anilino-ethylamino)-piperidine, which can be used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04144344uspto-grants-1979_03