Reaktion #1689769

ord-7f64737a9b324716abf769eab3f721b4

Reaktionsgleichung

COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O=C(O)C(O)C(O)C(=O)O
hydrocodone bitartrate
CCO
ethanol
→
COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O.O=C(O)[C@H](O)[C@@H](O)C(=O)O
final product
COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O.O=C(O)[C@H](O)[C@@H](O)C(=O)O
Hydrocodone Bitartrate Hemipentahydrate

Edukte

COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O=C(O)C(O)C(O)C(=O)O
hydrocodone bitartrate
CCO
ethanol

Reagenzien

Keine

Lösungsmittel

O
water
O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe sample was dried at 60° C. for 24 hours
  2. 2
    Sonstigeto afford 151.7 g of ethanol-free (as defined below) product

Vorschrift

A sample of 149.4 g of hydrocodone bitartrate containing 2.1 wt % of ethanol was placed in a crystallisation dish. The sample was placed in a vacuum oven along with a crystallisation dish containing water (ca 200 ml). A vacuum was applied (16665 pascals (approximately 10 mm to 1 mm Hg)) and the sample was dried at 60° C. for 24 hours to afford 151.7 g of ethanol-free (as defined below) product. The water content measured by Karl Fisher titration was 9.66% which indicated that the final product was a hemi-pentahydrate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05981751uspto-grants-1999_11