Hydrochloric Acid → 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid

HRID 1169336

Reaktionsgleichung

[CH2:1]([O:3][C:4]1[CH:26]=[CH:25][C:7]([CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]3[CH2:19][CH2:18][CH2:17][C:16]([C:20]([O:22]C)=[O:21])=[CH:15][C:14]=3[CH:24]=2)=[CH:6][CH:5]=1)[CH3:2].[OH-].[Na+].Cl>CO.C1COCC1>[CH2:1]([O:3][C:4]1[CH:26]=[CH:25][C:7]([CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]3[CH2:19][CH2:18][CH2:17][C:16]([C:20]([OH:22])=[O:21])=[CH:15][C:14]=3[CH:24]=2)=[CH:6][CH:5]=1)[CH3:2]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

To methyl 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate (296 mg, 0.84 mmol) dissolved in a mixed solvent of methanol (4 ml) and THF (4 ml) was added a 1N aqueous solution of sodium hydroxide (2.5 ml), and the resulting mixture was stirred at 50° C. for 4 hours. The reaction mixture was mixed with 1 N hydrochloric acid (2.5 ml) at 0° C., was concentrated under reduced pressure and was mixed with water, and an insoluble material was collected by filtration. The insoluble material was washed with water, and was dried under reduced pressure to obtain 2-(4-ethoxybenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid (283 mg, 0.84 mmol).

Aufarbeitung

concentrationwas concentrated under reduced pressure
additionwas mixed with water
filtrationan insoluble material was collected by filtration
washThe insoluble material was washed with water
customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-db514b2ce172494fa75877df27b187ac
Quelldatensatz: uspto-grants-2003_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06627651B1

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