Reaktion #576662

ord-abc2b6635b1f4a6e86074b49560ec630

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Wascheneluting with ethanol/hexane [40.60]

Vorschrift

A solution of (+)-3-bromocamphor-10-sulphonic acid (36.3 g, 0.110 moles) in IMS (40 ml) was added to a solution of the product of step (f) (50 g, 0.110 moles) in IMS (300 ml). After seeding, the resulting slurry was granulated for 20 hours at room temperature. A white solid (22 g, 0.03 moles) was collected by filtration after further granulating for 1 hour at low temperature. The chiral purity was assessed as 95% ee by chiral HPLC using a Chiralcel™ OD column and eluting with ethanol/hexane [40.60].

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06977302B2uspto-grants-2005_12