Hydrochloric Acid → Erlotinib hydrochloride

HRID 404534

Reaktionsgleichung

Reaktionsgleichung von HRID 404534
[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]>C(O)(C)C>[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

4

Edukt 2

HCID 313Hydrochloric AcidHCID 176870Erlotinib2×

Produkt 1

HCID 176871Erlotinib hydrochlorideAusbeute 91,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

Into a 1 Lt. four necked round-bottomed flask provided with a mechanical stirrer, thermometer socket, reflux condenser etc., are charged 325 mL of isopropyl alcohol, followed by 25.0 g of Erlotinib base (Prepared according to the process given in Example-(1) of PCT International Publication No. WO 2007/060691) at 70-75° C. so that Erlotinib base completely dissolves in the solvent. Then carbon treatment is given and the filtrate is transferred to another 1 Lt. four-necked round bottomed flask provided with all the necessary accessories. To this solution isoproponolic HCl (HCl content as 100% is 2.548 g) is added in one lot at 60-65° C. and maintained at this temperature for about 1 hour. The reaction mass is cooled to room temperature and filtered. The product is washed with fresh isopropyl alcohol and dried to get 25.0 g of Erlotinib hydrochloride as a white crystalline powder.

Aufarbeitung

  1. customfour necked round-bottomed flask provided with a mechanical stirrer
  2. temperaturethermometer socket, reflux condenser etc.
  3. customPrepared
  4. customfour-necked round bottomed flask provided with all the necessary accessories
  5. temperaturemaintained at this temperature for about 1 hour
  6. filtrationfiltered
  7. washThe product is washed with fresh isopropyl alcohol
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-69683049ff534bd4896aaa11134eeab0
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08748602B2

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