Hydrochloric Acid → Zantac

HRID 53912

Reaktionsgleichung

Reaktionsgleichung von HRID 53912
[CH3:1][N:2]([CH2:4][C:5]1[O:9][C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]([NH:20][CH3:21])=[CH:16][N+:17]([O-:19])=[O:18])=[CH:7][CH:6]=1)[CH3:3].[ClH:22]>C(O)CC>[CH3:21][NH:20][C:15]([NH:14][CH2:13][CH2:12][S:11][CH2:10][C:8]1[O:9][C:5]([CH2:4][N:2]([CH3:1])[CH3:3])=[CH:6][CH:7]=1)=[CH:16][N+:17]([O-:19])=[O:18].[ClH:22]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 5039Ranisen

Produkt 1

HCID 47909Zantac

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10311-PropanolLösungsmittel2×

Versuchsvorschrift

N-[2-[[[5-(Dimethylamino)methyl-2-furanyl]methyl]thio]ethyl]-N'-methyl-2-nitro-1,1-ethenediamine (5 g) was dissolved in n-propanol (20 ml). A further quantity of n-propanol (20 ml) containing molar equivalent of hydrogen chloride was added slowly to the solution. The solution was seeded with Form 1 crystals at this temperature to induce crystallization. It was stirred further for 1-2 hrs. The hydrochloride crystallized during this period, and was filtered off. The product was washed with n-propanol (2×5 ml) and was dried at 45° C. under vacuum to give Form 1 ranitidine hydrochloride (4.49 g), m.p. 136°-137° C., purity=99.6% (HPLC).

Aufarbeitung

  1. additionwas added slowly to the solution
  2. customcrystallization
  3. customThe hydrochloride crystallized during this period
  4. filtrationwas filtered off
  5. washThe product was washed with n-propanol (2×5 ml)
  6. customwas dried at 45° C. under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b71a0c91fa6e49fa944dc1a130dca624
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05621120

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