4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid methyl ester → 4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid
Reaktionsgleichung
C[O:2][C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:27]=[CH:26][C:15]3[CH2:16][CH2:17][N:18]([CH:21]4[CH2:25][CH2:24][CH2:23][CH2:22]4)[CH2:19][CH2:20][C:14]=3[CH:13]=2)=[CH:6][CH:5]=1>CO.[OH-].[Na+].O>[CH:21]1([N:18]2[CH2:19][CH2:20][C:14]3[CH:13]=[C:12]([O:11][CH2:10][C:7]4[CH:8]=[CH:9][C:4]([C:3]([OH:28])=[O:2])=[CH:5][CH:6]=4)[CH:27]=[CH:26][C:15]=3[CH2:16][CH2:17]2)[CH2:22][CH2:23][CH2:24][CH2:25]1Komponenten
5
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid methyl ester (E88) (3.1 g, 8.1 mmol)) was dissolved in a mixture of methanol (90 ml), 2N sodium hydroxide (12 ml) and water (30 ml). The resulting mixture was stirred at 60° C. for 4 hours and then cooled to room temperature. The mixture was concentrated in vacuo to remove the organic solvents and then acidified to pH 6 (2N hydrochloric acid). The resulting precipitates were filtered, washed with water and dried under vacuum to afford the title compound (E89); MS (ES+) m/e 366 [M+H]+.
Aufarbeitung
- temperaturecooled to room temperature
- concentrationThe mixture was concentrated in vacuo
- customto remove the organic solvents
- customThe resulting precipitates
- filtrationwere filtered
- washwashed with water
- customdried under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-efbe8f0d592a491cb01a194121e24f7f
- Quelldatensatz
- uspto-grants-2010_09
- Patentnummer
- US07799773B2
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