Doxazosin → Doxazosin Mesylate

HRID 1016365

Reaktionsgleichung

Reaktionsgleichung von HRID 1016365
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:19]([NH2:20])=[N:18][C:17]([N:21]3[CH2:26][CH2:25][N:24]([C:27]([CH:29]4[O:38][C:37]5[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=5[O:31][CH2:30]4)=[O:28])[CH2:23][CH2:22]3)=[N:16][C:11]2=[CH:12][C:13]=1[O:14][CH3:15]>CO>[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:19]([NH2:20])=[N:18][C:17]([N:21]3[CH2:22][CH2:23][N:24]([C:27]([CH:29]4[O:38][C:37]5[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=5[O:31][CH2:30]4)=[O:28])[CH2:25][CH2:26]3)=[N:16][C:11]2=[CH:12][C:13]=1[O:14][CH3:15].[CH3:1][S:2]([OH:5])(=[O:4])=[O:3]

Komponenten

4

Edukt 2

HCID 3157DoxazosinHCID 6395Methanesulfonic Acid2×

Produkt 1

HCID 62978Doxazosin MesylateAusbeute 148 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

17.7 g of anhydrous methanesulfonic acid were added to a stirred mixture of 79.0 g of doxazosin and 800 ml of methanol in a 2 1 three-necked round-bottomed flask. During this, the internal temperature rose to 30° C., and a solution formed. After the addition of the methanesulfonic acid was complete, the mixture was stirred for a further 5 h. The resulting precipitate was then filtered off with suction and washed 3× with 50 ml of methanol each time. 141.8 g of moist doxazosin mesylate (modification D) were obtained. This corresponds to 89.2 g of dry substance and a yield of 93.1%.

Aufarbeitung

  1. customrose to 30° C.
  2. customa solution formed
  3. filtrationThe resulting precipitate was then filtered off with suction
  4. washwashed 3× with 50 ml of methanol each time

Quellen und Nachweise

ORD-Eintrag
ord-67156bdc60da473a85c0a3f24026ebad
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06476033B1

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