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

HRID 3304

Reaktionsgleichung

Reaktionsgleichung von HRID 3304
[CH2:1]([C:4]1[CH:8]=[C:7]([C:9]23[CH2:16][CH2:15][CH2:14][N:13]2[CH2:12][CH2:11][CH2:10]3)[O:6][N:5]=1)[CH2:2][CH3:3].[ClH:17]>CCOCC>[ClH:17].[CH2:1]([C:4]1[CH:8]=[C:7]([C:9]23[CH2:10][CH2:11][CH2:12][N:13]2[CH2:14][CH2:15][CH2:16]3)[O:6][N:5]=1)[CH2:2][CH3:3]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 189347247a-(3-propyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine

Produkt 1

HCID 189347587a-(3-Propyl-5-isoxazolyl)-hexahydro-1h-pyrrolizine hydrochloride salt

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

7a-(3-propyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (265 mg, 1.30 mmol, from step 14a) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with Et2O and dried to afford the title compound as a free flowing white powder. mp 97°-98° C. MS (NH3 /CI): m/z 207 (M+H+); 1H NMR (D2O, 300 MHz) δ0.92 (t, J=7.5 Hz, 3H), 1.63-1.75 (m, 2H), 2.20-2.40 (m, 6H), 2.59-2.71 (m, 4H), 3.30-3.38 (m, 2H), 3.70-3.78,(m, 2H), 6.65 (s, 1H); MS (CI/NH3) m/z: 221 (M+H)+.Anal. Calcd for C13H20N2O.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 triturated with Et2O
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-402839b675474c22a8bd5c354e9adae4
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05733912

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