Reaktionsgleichung
[CH2:1]([C:3]1[CH:7]=[C:6]([C:8]23[CH2:15][CH2:14][CH2:13][N:12]2[CH2:11][CH2:10][CH2:9]3)[O:5][N:4]=1)[CH3:2].[ClH:16]>CCOCC>[ClH:16].[CH2:1]([C:3]1[CH:7]=[C:6]([C:8]23[CH2:15][CH2:14][CH2:13][N:12]2[CH2:11][CH2:10][CH2:9]3)[O:5][N:4]=1)[CH3:2]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
7a-(3-ethyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (265 mg, 1.30 mmol, from step 13b) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was recrystallized from methanol/ethanol to afford the title compound as a white solid: mp 139°-140° C.; 1H NMR D2O, 300 MHz) δ1.23 (t, J=7.5 Hz, 3H), 2.17-2.40 (m, 6H), 2.58-2.75 (m, 4H), 3.29-3.38 (m, 2H), 3.69-3.77 (m, 2H), 6.64 (s, 1H); MS (CI/NH3) m/z: 207 (M+H)+ ; Anal. Calcd for C12H18N2O.HCl: C, 59.38; H, 7.89; N, 11.54. Found: C, 59.44; H, 7.94; N, 11.48.
Aufarbeitung
- customThe solvent was removed
- customthe precipitate was recrystallized from methanol/ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-6a17fe06ca0a4559821af5872f757c00
- Quelldatensatz
- uspto-grants-1998_03
- Patentnummer
- US05733912
Verknüpfte Notizen
Wird geladen…