Maleic Acid → GSK-2245035 maleate

HRID 2367968Notizen

Reaktionsgleichung

[NH2:1][C:2]1[N:10]=[C:9]([O:11][C@@H:12]([CH3:16])[CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:28])[N:6]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1.[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]\[C:32]([OH:34])=[O:33]>C(O)(C)C>[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]\[C:32]([OH:34])=[O:33].[NH2:1][C:2]1[N:10]=[C:9]([O:11][C@@H:12]([CH3:16])[CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:28])[N:6]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]1

Komponenten

Reaktionsbedingungen

Temperatur: 40 °C

Versuchsvorschrift

6-amino-2-{[(1S)-1-methylbutyl]oxy}-9-[5-(1-piperidinyl)pentyl]-7,9-dihydro-8H-purin-8-one (for example, as prepared for Reference Example 1) (0.384 g, 0.98 mmol) was dissolved in isopropyl alcohol (4.6 mL, 12 vols) and heated to 40° C. Maleic acid (0.114 g, 0.98 mmol) was added. A clear solution was obtained. During cooling to room temperature, precipitation occurred. The slurry was filtered, washing with isopropyl alcohol (5 mL) and dried under reduced pressure at 40° C. to constant weight. 6-amino-2-{[(1S)-1-methylbutyl]oxy}-9-[5-(1-piperidinyl)pentyl]-7,9-dihydro-8H-purin-8-one, maleate salt (0.305 g, 61% th) was obtained as a white solid.

Aufarbeitung

customA clear solution was obtained
temperatureDuring cooling to room temperature
customprecipitation
filtrationThe slurry was filtered
washwashing with isopropyl alcohol (5 mL)
customdried under reduced pressure at 40° C. to constant weight

Quellen und Nachweise

ORD-Eintrag: ord-272fe083014a41e19c4783dd6e94a8a3
Quelldatensatz: uspto-grants-2014_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08703754B2

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