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Hydrochloric Acid → Carvedilol phosphate monohydrate

HRID 2358166
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2358166
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=1[O:9][CH2:10][CH2:11][NH:12][CH2:13][CH:14]([OH:30])[CH2:15][O:16][C:17]1[CH:18]=[CH:19][CH:20]=[C:21]2[NH:29][C:28]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:22]=12.O.[P:32]([O-:36])([O-:35])([OH:34])=[O:33].[K+].[K+].Cl>CC(C)=O>[CH3:1][O:2][C:3]1[C:8]([O:9][CH2:10][CH2:11][NH:12][CH2:13][CH:14]([OH:30])[CH2:15][O:16][C:17]2[C:22]3[C:23]4[C:28]([NH:29][C:21]=3[CH:20]=[CH:19][CH:18]=2)=[CH:27][CH:26]=[CH:25][CH:24]=4)=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH2:33].[OH:34][P:32]([OH:36])([OH:35])=[O:33]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 2585CarvedilolHCID 24450Potassium Phosphate, Dibasic

Produkt 1

HCID 23649704Carvedilol phosphate monohydrateAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180
Acetone
Lösungsmittel

Reaktionsbedingungen

Temperatur
32.5 °C

Versuchsvorschrift

Carvedilol (15 gm, 0.0375M), water (240 ml, 13.33M) and dipotassium hydrogen orthophosphate (6.5 g, 0.0375M) were charged in to a reactor and stirred for 10 minutes at 30-35° C. Cooled the reaction mass to 5-10° C. The pH of the reaction mass was adjusted to 4.5-5 with hydrochloric acid. The temperature was raised to 50-55° C. Acetone (51 ml, 0.7M) was added and stirred at 50-55° C. for two hours. Reaction mass was cooled to 30-35° C. and stirred for 24 hours. The reaction mass was further cooled to 5-10° C. and maintained for 1 hour. Carvedilol dihydrogen phosphate monohydrate was filtered, washed with water, suck dried and dried under vacuum at 40-45° C. till constant weight to obtain carvedilol phosphate monohydrate.

Aufarbeitung

  1. temperatureCooled the reaction mass to 5-10° C
  2. temperatureThe temperature was raised to 50-55° C
  3. stirringstirred at 50-55° C. for two hours
  4. customReaction mass
  5. temperaturewas cooled to 30-35° C.
  6. stirringstirred for 24 hours
  7. temperatureThe reaction mass was further cooled to 5-10° C.
  8. temperaturemaintained for 1 hour
  9. filtrationCarvedilol dihydrogen phosphate monohydrate was filtered
  10. washwashed with water, suck
  11. customdried
  12. customdried under vacuum at 40-45° C. till constant weight

Quellen und Nachweise

ORD-Eintrag
ord-728c1bc3482d44bbb5315b67f00a71ee
Quelldatensatz
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07763645B2

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