Terazosin Hydrochloride → Terazosin

HRID 2379400

Reaktionsgleichung

Reaktionsgleichung von HRID 2379400
[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[C:9]([NH2:26])=[N:10][C:11]([N:13]3[CH2:18][CH2:17][N:16]([C:19]([CH:21]4[O:25][CH2:24][CH2:23][CH2:22]4)=[O:20])[CH2:15][CH2:14]3)=[N:12][C:6]2=[CH:5][C:4]=1[O:27][CH3:28].O.O.Cl>CC(C)=O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[C:9]([NH2:26])=[N:10][C:11]([N:13]3[CH2:18][CH2:17][N:16]([C:19]([CH:21]4[O:25][CH2:24][CH2:23][CH2:22]4)=[O:20])[CH2:15][CH2:14]3)=[N:12][C:6]2=[CH:5][C:4]=1[O:27][CH3:28]

Komponenten

3

Edukt 1

HCID 63016Terazosin Hydrochloride

Produkt 1

HCID 5401TerazosinAusbeute 90,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To a 500-mL round-bottom flask containing 5.19 g (0.011 mol) of terazosin monohydrochloride dihydrate was added 250 mL of dry acetone and several glass boiling beads. The flask was fitted with a Dean-Stark trap and reflux condensor. The heterogenous mixture was heated under reflux for five days. After cooling, the undissolved white solid remaining in the flask was collected by vacuum filtration to yield 4.3 g (0.010 mol, 90.9% yield) of the anhydrous crystalline polymorph of terazosin of this invention. The material was found by its powder x-ray diffraction pattern to be free of both the prior art anhydrous crystalline modification and the dihydrate form.

Aufarbeitung

  1. customThe flask was fitted with a Dean-Stark trap
  2. temperaturereflux condensor
  3. temperatureThe heterogenous mixture was heated
  4. temperatureunder reflux for five days
  5. temperatureAfter cooling
  6. filtrationwas collected by vacuum filtration

Quellen und Nachweise

ORD-Eintrag
ord-c7aa683dcf7d443886995c02b7c0e72e
Quelldatensatz
uspto-grants-1994_11
Patentnummer
US05362730

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