Reaktion #84048

ord-0186fe48a824439e807128658024c08c

Reaktionsgleichung

Cl.O=C1CN2CCC1CC2
quinuclidin-3-one hydrochloride
C[O-].[Na+]
sodium methoxide
O=C1CN2CCC1CC2
title compound
O=C1CN2CCC1CC2
Quinuclidin-3-one

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe resulting precipitate is filtered off with suction
  2. 2
    Einengenthe filtrate is concentrated in vacuo
  3. 3
    SonstigeThe residue is partitioned between chloroform and water
  4. 4
    Extraktionextracted with chloroform
  5. 5
    TrocknenThe combined organic phases are dried over sodium sulfate
  6. 6
    Einengenconcentrated in vacuo

Vorschrift

100 g (0.62 mol) of quinuclidin-3-one hydrochloride are suspended in 2 l of methanol. At 0° C., a solution of 33.4 g (0.62 mol) of sodium methoxide in 250 ml of methanol is slowly added dropwise. The mixture is stirred at room temperature for 16 h. The resulting precipitate is filtered off with suction, and the filtrate is concentrated in vacuo. The residue is partitioned between chloroform and water and extracted with chloroform. The combined organic phases are dried over sodium sulfate and concentrated in vacuo. 58.8 g (75.9% of theory) of the title compound are obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09433614B2uspto-grants-2016_09