Reaktion #674315

ord-645bf87f5737445791c0f383d910c826

Reaktionsgleichung

COC(=O)C(c1ccccc1)C1CCCCN1.Cl
methylphenidate hydrochloride
[NH4+].[OH-]
Ammonium hydroxide
COC(=O)[C@H](c1ccccc1)[C@H]1CCCCN1
oil
Ausbeute 98.0%
COC(=O)[C@H](c1ccccc1)[C@H]1CCCCN1
d-Methylphenidate
Ausbeute 98.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeformed
  2. 2
    ExtraktionThe product was extracted with three 100 mL portions of ethyl acetate
  3. 3
    Trocknenthe combined organic layers were dried over sodium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated
  6. 6
    Sonstigeat 40° C.

Vorschrift

To a 200 mL beaker was charged 10.0 g (37.1 mmol) racemic-methylphenidate hydrochloride and 135 mL water. Ammonium hydroxide (3.40 g; 96.8 mmol) was then added to bring the pH to approximately 9 upon which an oily semi-solid formed. The product was extracted with three 100 mL portions of ethyl acetate, the combined organic layers were dried over sodium sulfate, filtered and concentrated under reduce pressure at 40° C. to provide 8.5 g of a clear, colorless viscous oil (98% yield). The free base was characterized by FTIR and found to be consistent with the anticipated structure

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09226925B1uspto-grants-2016_01