Hydrochloric Acid → 2-[(tetrahydropyran-4-yl)oxy]-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid

HRID 1169347Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1169347
[O:1]1[CH2:6][CH2:5][CH:4]([O:7][C:8]2[CH:9]=[CH:10][C:11]3[CH2:17][CH2:16][CH2:15][C:14]([C:18]([O:20]C)=[O:19])=[CH:13][C:12]=3[CH:22]=2)[CH2:3][CH2:2]1.[OH-].[Na+].Cl>CO.C1COCC1>[O:1]1[CH2:2][CH2:3][CH:4]([O:7][C:8]2[CH:9]=[CH:10][C:11]3[CH2:17][CH2:16][CH2:15][C:14]([C:18]([OH:20])=[O:19])=[CH:13][C:12]=3[CH:22]=2)[CH2:5][CH2:6]1

Komponenten

6

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To methyl 2-[(tetrahydropyran-4-yl)oxy]-6,7-dihydro-5H-benzocycloheptene-8-carboxylate (406 mg, 1.34 mmol) dissolved in a mixed solvent of methanol (7 ml) and THF (7 ml) was added a 1N aqueous solution of sodium hydroxide (4.0 ml), and the resulting mixture was stirred at 60° C. for 5 hours. The reaction mixture was mixed with 1 N hydrochloric acid (4.0 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-[(tetrahydropyran-4-yl)oxy]-6,7-dihydro-5H-benzocycloheptene-8-carboxylic acid (307 mg, 1.28 mmol, 96%).

Aufarbeitung

  1. concentrationwas concentrated under reduced pressure
  2. additionwas mixed with water
  3. filtrationan insoluble material was collected by filtration
  4. washThe insoluble material was washed with water
  5. customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-926bb25af7f04423b7ba94d1639b0ceb
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06627651B1

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