Hydrochloric Acid → Erlotinib hydrochloride

HRID 404533

Reaktionsgleichung

[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[C:10]2[C:12]([NH:16][C:17]3[CH:22]=[C:21]([C:23]#[CH:24])[CH:20]=[CH:19][CH:18]=3)=[N:13][CH:14]=[N:15][C:9]2=[CH:8][C:7]=1[O:25][CH2:26][CH2:27][O:28][CH3:29].[ClH:30]>CO>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[C:10]2[C:12]([NH:16][C:17]3[CH:18]=[CH:19][CH:20]=[C:21]([C:23]#[CH:24])[CH:22]=3)=[N:13][CH:14]=[N:15][C:9]2=[CH:8][C:7]=1[O:25][CH2:26][CH2:27][O:28][CH3:29].[ClH:30]

Komponenten

Reaktionsbedingungen

Temperatur: 32.5 °C

Versuchsvorschrift

Into a 2 Lt. four necked round-bottomed flask provided with a mechanical stirrer, thermometer socket, reflux condenser etc., are charged 1340 mL of methanol, followed by Erlotinib base 60 g. (Prepared according to the process given in Example-(1) of PCT International Publication No. WO 2007/060691). The reaction mass is warmed to around 40° C. so that Erlotinib base completely dissolves. To this reaction mass, carbon treatment is given and the filtrate is transferred to another 2 Lt. four necked flask. To this solution isopropanolic HCl (HCl content as 100% is 6.12 g) is added in one lot and the reaction mass is stirred at 30-35° C. for about 90 minutes and filtered. The product is washed with fresh methanol and dried the wet cake to get 55.2 g of Erlotinib hydrochloride as a white crystalline powder.

Aufarbeitung

customfour necked round-bottomed flask provided with a mechanical stirrer
temperaturethermometer socket, reflux condenser etc.
custom(Prepared
customThe reaction
dissolutioncompletely dissolves
filtrationfiltered
washThe product is washed with fresh methanol
customdried the wet cake

Quellen und Nachweise

ORD-Eintrag: ord-9106fa1dbe6e4bf3b36718b48813247e
Quelldatensatz: uspto-grants-2014_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08748602B2

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