Nefazodone → Nefazodone hydrochloride

HRID 1636233

Reaktionsgleichung

Reaktionsgleichung von HRID 1636233
[CH3:1][CH2:2][C:3]1[N:8]([CH2:9][CH2:10][O:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:6](=[O:7])[N:5]([CH2:18][CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][N:24]([C:27]3[CH:28]=[CH:29][CH:30]=[C:31]([Cl:33])[CH:32]=3)[CH2:23][CH2:22]2)[N:4]=1.[OH-].[Na+]>O>[CH3:1][CH2:2][C:3]1[N:8]([CH2:9][CH2:10][O:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:6](=[O:7])[N:5]([CH2:18][CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][N:24]([C:27]3[CH:28]=[CH:29][CH:30]=[C:31]([Cl:33])[CH:32]=3)[CH2:23][CH2:22]2)[N:4]=1.[ClH:33]

Komponenten

4

Edukt 2

HCID 4449NefazodoneHCID 14798Sodium Hydroxide

Produkt 1

HCID 54911Nefazodone hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
42.5 °C

Versuchsvorschrift

Nefazodone HCl was prepared in accordance with Example 2 of U.S. Pat. No. 4,338,317. Nefazodone HCI was dissolved in water with gentle heating (40-45° C.). An equimolar quantity of sodium hydroxide solution (0.1 N) was added with constant stirring while cooling with ice. Nefazodone base precipitated as a sticky gum which was separated and washed repeatedly with water. The base was washed with water until no chloride ions (AgNO3 test) were detected in the washings. Nefazodone base was then dissolved and crystallized from isopropyl alcohol (IPA) to give a solid melting 81-83° C.

Aufarbeitung

  1. temperaturewhile cooling with ice
  2. customNefazodone base precipitated as a sticky gum which
  3. customwas separated
  4. washwashed repeatedly with water
  5. washThe base was washed with water until no chloride ions (AgNO3 test)
  6. dissolutionNefazodone base was then dissolved
  7. customcrystallized from isopropyl alcohol (IPA)
  8. customto give a solid
  9. custommelting 81-83° C.

Quellen und Nachweise

ORD-Eintrag
ord-02174f92564844058b99dde18f2e5844
Quelldatensatz
uspto-grants-2000_03
Patentnummer
US06034085

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