Sodium Hydroxide → Sunitinib

HRID 84785

Reaktionsgleichung

Reaktionsgleichung von HRID 84785
[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:12]([CH3:29])=[C:13](/[CH:17]=[C:18]2/[C:19]3[CH:20]=[C:21]([F:28])[CH:22]=[CH:23][C:24]=3[NH:25][C:26]/2=[O:27])[NH:14][C:15]=1[CH3:16])=[O:10])[CH2:4][CH3:5].CS([O-])(=O)=O.[OH-].[Na+]>O>[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:12]([CH3:29])=[C:13](/[CH:17]=[C:18]2/[C:19]3[CH:20]=[C:21]([F:28])[CH:22]=[CH:23][C:24]=3[NH:25][C:26]/2=[O:27])[NH:14][C:15]=1[CH3:16])=[O:10])[CH2:4][CH3:5]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 86691059Sunitinib methanesulfonate

Produkt 1

HCID 5329102SunitinibAusbeute 99,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

Sunitinib methanesulfonate (1.0 g) and H2O (60 mL) was added into a flask in r.t. and heated to 80° C., the mixture turned clear. The pH of the mixture was adjusted to 8˜9 with 1N NaOH and cooled r.t., was stirred overnight, filtered, washed, and dried in vacuo to give 0.65 g of crude sunitinib with 99.2% purity by HPLC analysis in 99.5% yield.

Aufarbeitung

  1. temperaturecooled r.t.
  2. filtrationfiltered
  3. washwashed
  4. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b24cd80ef32e41859a7e5c7bd4853404
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846953B2

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