Hydrochloric Acid → 7a-(4-Methyl-3-pyridinyl)-hexahydro-1h-pyrrolizine dihydrochloride salt

HRID 3330Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 3330
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]12[CH2:15][CH2:14][CH2:13][N:12]1[CH2:11][CH2:10][CH2:9]2.[ClH:16]>CCOCC>[ClH:16].[ClH:16].[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]12[CH2:15][CH2:14][CH2:13][N:12]1[CH2:11][CH2:10][CH2:9]2

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 189347417a-(4-methyl-3-pyridinyl)-hexahydro-1H-pyrrolizine

Produkt 1

HCID 189347407a-(4-Methyl-3-pyridinyl)-hexahydro-1h-pyrrolizine dihydrochloride saltAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

7a-(4-methyl-3-pyridinyl)-hexahydro-1H-pyrrolizine (37 mg, 0.18 mmol) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the solid was triturated with Et2O and dried to afford the title compound as a white solid (26.2 mg, 61%): mp 244°-247° C.; 1H NMR D2O, 300 MHz) δ2.01-2.16 (m, 2H), 2.27-2.52 (m, 4H), 2.65 (s, 3H), 2.65-2.78 (m, 2H), 3.45-3.54 (m, 2H), 3.87-3.96 (m, 2H), 7.75 (d, J=5.6 Hz, 1H), 8.49 (s, 1H), 8.55 (d, J=5.6 Hz, 1H); MS (CI/NH3): m/z 203 (M+H+). Anal. Calcd for C13H18N2.2 HCl: C, 56.73; H, 7.32; N, 10.18. Found: C, 56.94; H. 7.24; N, 9.99.

Aufarbeitung

  1. customThe solvent was removed
  2. customthe solid was triturated with Et2O
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9f0d302e51834ee5ae59f2e30cfe7ffc
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05733912

Notizen zur Reaktion

Wird geladen…