Methanesulfonic Acid → Rasagiline mesylate

HRID 401853Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 401853
[CH:1]#[C:2][CH2:3][NH:4][C@H:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6]1.[CH3:14][S:15]([OH:18])(=[O:17])=[O:16]>CC(O)C>[CH3:14][S:15]([OH:18])(=[O:17])=[O:16].[CH:1]#[C:2][CH2:3][NH:4][C@H:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6]1

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 3052776Rasagiline

Produkt 1

HCID 3052775Rasagiline mesylateAusbeute 83,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

Rasagiline base (81 g, 0.47 moles) was dissolved in IPA (810 ml) under stirring and the obtained solution was cooled to 5° C. A solution of methanesulfonic acid (0.49 moles, 47.7 g) in IPA (95 ml) was added dropwise to the above cooled solution. After complete addition, the mixture was stirred for 30 min at 5-10° C. to get the solid which was filtered and dried to get (105 g, 83%) of Rasagiline mesylate.

Aufarbeitung

  1. additionAfter complete addition
  2. stirringthe mixture was stirred for 30 min at 5-10° C.
  3. customto get the solid which
  4. filtrationwas filtered
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3ba668adc1934c91ba8d932d1597670e
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08741962B2

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