Hydrochloric Acid → HCID 67232788, Verbindung
Reaktionsgleichung
[CH3:1][C:2]1([CH3:30])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]([NH:13][CH2:14][CH:15]2[CH2:20][CH2:19][N:18]([CH2:21][C:22]3([C:26]([OH:28])=[O:27])[CH2:25][CH2:24][CH2:23]3)[CH2:17][CH2:16]2)=[O:12])[C:3]1=[O:29].[ClH:31]>O1CCCC1>[ClH:31].[CH3:1][C:2]1([CH3:30])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]([NH:13][CH2:14][CH:15]2[CH2:20][CH2:19][N:18]([CH2:21][C:22]3([C:26]([OH:28])=[O:27])[CH2:25][CH2:24][CH2:23]3)[CH2:17][CH2:16]2)=[O:12])[C:3]1=[O:29]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 45 °C
Versuchsvorschrift
1-{[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1h-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid (41.0 g, 99.2 mmol, Example 9) was dissolved with tetrahydrofuran (820 mL). The mixture was filtered and washed with tetrahydrofuran (410 mL) and the resulting solution was heated to 45° C. Aqueous concentrated hydrogen chloride (12N, 8.27 mL, 99.2 mmol) was added to the solution at 45° C. for 20 min and stirred at this temperature for 1 h. The suspension was cooled to 20° C. for 1 min stirred at 2 h. After filtration, the resulting solid was washed with tetrahydrofuran (205 mL), and dried in vacuo at 40° C. The titled compound was obtained as white solid (38.6 g, 86.6%)
Aufarbeitung
- filtrationThe mixture was filtered
- washwashed with tetrahydrofuran (410 mL)
- temperatureThe suspension was cooled to 20° C. for 1 min
- stirringstirred at 2 h
- filtrationAfter filtration
- washthe resulting solid was washed with tetrahydrofuran (205 mL)
- customdried in vacuo at 40° C
Quellen und Nachweise
- ORD-Eintrag
- ord-a3ad91ba5be84d86a5e42aca7b5db3ba
- Quelldatensatz
- uspto-grants-2009_09
- Patentnummer
- US07589109B2
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