Hydrochloric Acid → 7-(4-Methoxyphenyl)-2,3-dihydro-1-benzo-thiepine-4-carboxylic acid

HRID 1388008Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1388008
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18][CH2:17][CH2:16][C:15]([C:19]([O:21]C)=[O:20])=[CH:14][C:13]=3[CH:23]=2)=[CH:5][CH:4]=1.[OH-].[Na+].Cl>C(O)C.C1COCC1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18][CH2:17][CH2:16][C:15]([C:19]([OH:21])=[O:20])=[CH:14][C:13]=3[CH:23]=2)=[CH:5][CH:4]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18472336Methyl 7-(4-methoxyphenyl)-2,3-dihydro-1-benzothiepine-4-carboxylate

Produkt 1

HCID 184723977-(4-Methoxyphenyl)-2,3-dihydro-1-benzo-thiepine-4-carboxylic acidAusbeute 106,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21873804Tetrahydrofuran ethanolLösungsmittel

Versuchsvorschrift

To a solution of methyl 7-(4-methoxyphenyl)-2,3-dihydro-1-benzothiepine-4-carboxylate (0.50 g) in ethanol/THF (10/10 ml) was added at room temperature 1N sodium hydroxide solution (2 ml), and the mixture was stirred for 18 hours. To the mixture was added 1N hydrochloric acid (2 ml). Under reduced pressure, the mixture was concentrated. To the mixture was added water, and the precipitates were collected by filtration, which were washed with 2-propanol, diethylether and hexane to give pale yellow solid of 7-(4-methoxyphenyl)-2,3-dihydro-1-benzo-thiepine-4-carboxylic acid (508 mg). This compound was used for the following reaction, without subjecting further purification.

Aufarbeitung

  1. concentrationUnder reduced pressure, the mixture was concentrated
  2. additionTo the mixture was added water
  3. filtrationthe precipitates were collected by filtration, which
  4. washwere washed with 2-propanol, diethylether and hexane

Quellen und Nachweise

ORD-Eintrag
ord-ff44dcfb401544db96f8920fb65c6115
Quelldatensatz
uspto-grants-2001_07
Patentnummer
US06268354B1

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