Hydrochloric Acid → HCID 67521251, Verbindung

HRID 1926036Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1926036
[Cl:1][C:2]1[CH:3]=[C:4]([NH:17][C:18]2[C:19]3[NH:26][C:25]([CH2:27][NH:28]C(=O)OC(C)(C)C)=[CH:24][C:20]=3[N:21]=[CH:22][N:23]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=1.[ClH:36].C(O)C>O1CCCC1>[ClH:1].[ClH:36].[NH2:28][CH2:27][C:25]1[NH:26][C:19]2[C:18]([NH:17][C:4]3[CH:5]=[CH:6][C:7]([O:8][CH2:9][C:10]4[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=4)=[C:2]([Cl:1])[CH:3]=3)=[N:23][CH:22]=[N:21][C:20]=2[CH:24]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 86626249Carbamic acid, N-[[4-[[3-chloro-4-[(3-fluorophenyl)methoxy]phenyl]amino]-5H-pyrrolo[3,2-d]pyrimidin-6-yl]methyl]-, 1,1-dimethylethyl ester

Produkt 1

HCID 67521251HCID 67521251, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of tert-butyl [4-({3-chloro-4-[(3-fluorobenzyl)oxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-6-yl]methylcarbamate (500 mg) in tetrahydrofuran (12 mL) was added 2N hydrochloric acid (6.0 mL) at room temperature. The mixture was stirred at 60° C. for 2 hrs, ethanol was added to the reaction system and the mixture was concentrated under reduced pressure. The resultant crystals were collected by filtration and washed with diisopropyl ether to give the title compound (481.4 mg) as pale-yellow powder crystals.

Aufarbeitung

  1. concentrationthe mixture was concentrated under reduced pressure
  2. filtrationThe resultant crystals were collected by filtration
  3. washwashed with diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-30aea98815ec4dfab332a9050ef94603
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08178543B2

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