Reaktion #1994226

Reaktionsgleichung

Boc-Gly Rotigotine HCl

trifluoroacetic acid

→

Gly Rotigotine

Ausbeute 79.0%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeall the volatiles were removed
2. 2
   Sonstigea rotary evaporator
3. 3
   workup.DISSOLUTIONThe residue (dark yellow) was dissolved in methanol
4. 4
   Sonstigeprecipitated
5. 5
   workup.ADDITIONby adding into diethyl ether (40 mL)
6. 6
   FiltrationThe pale yellow precipitate was filtered
7. 7
   Sonstigedried

Vorschrift

The Boc-Gly-Rotigotine HCl was deprotected by first dissolving the product (1.258 g, 2.55 mmol) in dichloromethane (64 ml). After addition of trifluoroacetic acid (9.83 ml, 128 mmol), the reaction mixture was stirred for 1 hour at room temperature and then all the volatiles were removed using a rotary evaporator. The residue (dark yellow) was dissolved in methanol and precipitated by adding into diethyl ether (40 mL). The pale yellow precipitate was filtered using a glass frit and dried to give Gly-Rotigotine.2TFA (1.140 g, 79% yield).

Quelle