methyl (S)-phenyl((R)-piperidin-2-yl)acetate → Dexmethylphenidate

HRID 599388

Reaktionsgleichung

[CH3:1][O:2][C:3]([C@@H:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C@@H:6]1[NH:11][CH2:10][CH2:9][CH2:8][CH2:7]1)=[O:4]>O>[CH3:1][O:2][C:3]([C@H:5]([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[C@@H:6]1[NH:11][CH2:10][CH2:9][CH2:8][CH2:7]1)=[O:4]

Komponenten

Reaktionsbedingungen

Temperatur: 47.5 °C

Versuchsvorschrift

The chiral resolution generally proceeds by initially charging the racemic threo-methylphenidate, chiral acid and lower alkanol to a suitable reactor under agitation and ambient conditions. The base is then charged at a temperature ranging from about 20 to 30° C., and the resulting slurry is heated to an effective temperature, such as about 40 to 55° C. Process water is then charged and the mixture may be aged, such as aging at 40 to 45° C. for an effective amount of time, such as from about 15 minute to 1 hour. The heated resolution mixture is then cooled to a temperature and for a time effective to precipitate the d-threo-methylphenidate chiral acid salt. For example, the reaction can be cooled to about 0 to 25° C. over the course of approximately 1 to 3 hours and then aged at about 0 to 25° C. for about 1 to 3 hours. The precipitated d-threo methylphenidate/chiral acid salt is then isolated, such as by filtration.

Aufarbeitung

additionThe base is then charged at a temperature
customranging from about 20 to 30° C.
customas aging at 40 to 45° C. for an effective amount of time, such as from about 15 minute to 1 hour
temperatureThe heated resolution mixture is then cooled to a temperature and for a time effective
customto precipitate the d-threo-methylphenidate chiral acid salt
temperaturecan be cooled to about 0 to 25° C. over the course of approximately 1 to 3 hours

Quellen und Nachweise

ORD-Eintrag: ord-d8ccdc889df3419d9753ca020232c820
Quelldatensatz: uspto-grants-2011_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07897777B2

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