Hydrochloric Acid → 7a-(2,6-Dichloro-3-pyridinyl)-hexahydro-1h-pyrrolizine hydrochloride salt

HRID 3296Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 3296
[Cl:1][C:2]1[C:7]([C:8]23[CH2:15][CH2:14][CH2:13][N:12]2[CH2:11][CH2:10][CH2:9]3)=[CH:6][CH:5]=[C:4]([Cl:16])[N:3]=1.Cl>CCOCC>[ClH:1].[Cl:1][C:2]1[C:7]([C:8]23[CH2:9][CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][CH2:15]3)=[CH:6][CH:5]=[C:4]([Cl:16])[N:3]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 189347197a-(2,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine

Produkt 1

HCID 189347667a-(2,6-Dichloro-3-pyridinyl)-hexahydro-1h-pyrrolizine hydrochloride saltAusbeute 101 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

7a-(2,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 11a, 62 mg, 0.24 mmol) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with Et2O to give a white solid (35.6 mg). mp 212°-214° C. 1H NMR D2O, 300 MHz) δ2.02-2.18 (m, 2H), 2.28-2.41 (m, 2H), 2.52-2.64 (m, 2H), 2.72-2.83 (m, 2H), 3.41-3.50 (m, 2H), 3.92-4.02 (m, 2H), 7.60 (d, J=8.5 Hz, 1H), 8.00 (d, J=8.5 Hz, 1H); MS (ClfNH3) m/z: 257/259 (M+H)+. Anal. Calcd for C12 H16ClFN2 : C, 49.26; H, 4.82; N, 9.57. Found: C, 49.14; H, 5.03; N, 9.47.

Aufarbeitung

  1. customThe solvent was removed
  2. customthe precipitate was triturated with Et2O

Quellen und Nachweise

ORD-Eintrag
ord-6a4ede5955b04d74b49bc94baae656f9
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05733912

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