Hydrochloric Acid → 7-(4-Tert-butylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid
Reaktionsgleichung
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[S:20](=[O:22])(=[O:21])[CH2:19][CH2:18][C:17]([C:23]([O:25]C)=[O:24])=[CH:16][C:15]=3[CH:27]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl>COCCOC>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[S:20](=[O:21])(=[O:22])[CH2:19][CH2:18][C:17]([C:23]([OH:25])=[O:24])=[CH:16][C:15]=3[CH:27]=2)=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
To a solution of methyl 7-(4-tert-butylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (400 mg) in 1,2-dimethoxyethane (20 ml) was added 6N hydrochloric acid (10 ml), and the mixture was stirred at 70° C. for 55 hours, cooled to room temperature and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give crystals, which were collected by filtration and washed with hexane to give pale yellow crystals of 7-(4-tert-butylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (362.7 mg).
Aufarbeitung
- temperaturecooled to room temperature
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried with magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give crystals, which
- filtrationwere collected by filtration
- washwashed with hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-9657dde74d844340ac2de3302419fca8
- Quelldatensatz
- uspto-grants-2001_05
- Patentnummer
- US06235771B1
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