Hydrochloric Acid → 7a-(3-Ethyl-5-isoxazolyl)-hexahydro-1h-pyrrolizine hydrochloride salt

HRID 3302

Reaktionsgleichung

Reaktionsgleichung von HRID 3302
[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

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

  1. customThe solvent was removed
  2. customthe precipitate was recrystallized from methanol/ethanol

Quellen und Nachweise

ORD-Eintrag
ord-6a17fe06ca0a4559821af5872f757c00
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05733912

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