Hydrochloric Acid → Erlotinib hydrochloride

HRID 243532

Reaktionsgleichung

Reaktionsgleichung von HRID 243532
[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].O1CCOCC1.[ClH:36]>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:36]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 176870Erlotinib

Produkt 1

HCID 176871Erlotinib hydrochlorideAusbeute 97,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

10.0 g crystal form IV of erlotinib base was added to 200 ml 1,4-dioxane, heated to dissolve until being clarified, 6.4 g isopropanol saturated with HCl gas was added dropwise at 60-70° C., after dripping, stirred for 30 minutes while maintaining the temperature, stirred for 1 hour at 0-15° C. before filtration, dried at 50° C. to obtain 10.6 g sample of crystal form A. The yield was 97.2% and the purity was 99.8% (by HPLC).

Aufarbeitung

  1. temperatureheated
  2. dissolutionto dissolve
  3. temperaturewhile maintaining the temperature
  4. stirringstirred for 1 hour at 0-15° C. before filtration
  5. customdried at 50° C.
  6. customto obtain 10.6 g sample of crystal form A

Quellen und Nachweise

ORD-Eintrag
ord-6190bf32fedb433b972574d6bf7167e2
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08653264B2

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