Hydrochloric Acid → Zolpidem hydrochloride

HRID 1066183

Reaktionsgleichung

Reaktionsgleichung von HRID 1066183
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:16]=[C:15]3[N:10]([CH:11]=[C:12]([CH3:17])[CH:13]=[CH:14]3)[C:9]=2[CH2:18][C:19]([N:21]([CH3:23])[CH3:22])=[O:20])=[CH:6][CH:7]=1.[ClH:24]>C(O)CCC>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:16]=[C:15]3[N:10]([CH:11]=[C:12]([CH3:17])[CH:13]=[CH:14]3)[C:9]=2[CH2:18][C:19]([N:21]([CH3:22])[CH3:23])=[O:20])=[CH:4][CH:3]=1.[ClH:24]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 5732Zolpidem

Produkt 1

HCID 18004031Zolpidem hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

One gram of zolpidem is suspended in 35 ml of 1-butanol, 0.32 g of concentrated hydrochloric acid is added and the mixture stirred 15 minutes at room temperature. The clear solution is heated to reflux and 25 ml of a water/1-butanol mixture is distilled off. The resulting mixture is allowed to cool to room temperature and stirred at room temperature for 16 hours. The formed solid is filtered off, washed with 2 ml of 1-butanol and dried in a vacuum oven at 40° C. to produce zolpidem hydrochloride anhydrate. A representative DSC curve is shown in FIG. 11.

Aufarbeitung

  1. temperatureThe clear solution is heated
  2. temperatureto reflux
  3. distillation25 ml of a water/1-butanol mixture is distilled off
  4. temperatureto cool to room temperature
  5. stirringstirred at room temperature for 16 hours
  6. filtrationThe formed solid is filtered off
  7. washwashed with 2 ml of 1-butanol
  8. customdried in a vacuum oven at 40° C.

Quellen und Nachweise

ORD-Eintrag
ord-867bfc6d27514615bf014daebcce4be2
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06242460B1

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