HCID 18472481, Verbindung → HCID 18472317, Verbindung

HRID 2228281Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2228281
[CH3:1][C:2]1[CH:3]=[C:4]([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][C:13]([C:17]([O:19]C)=[O:18])=[CH:12][C:11]=3[CH:21]=2)[S:5][CH:6]=1>C1COCC1.[OH-].[Na+]>[CH3:1][C:2]1[CH:3]=[C:4]([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][C:13]([C:17]([OH:19])=[O:18])=[CH:12][C:11]=3[CH:21]=2)[S:5][CH:6]=1

Komponenten

4

Edukt 1

HCID 18472481HCID 18472481, Verbindung

Produkt 1

HCID 18472317HCID 18472317, VerbindungAusbeute 79,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

In THF (10 ml) was dissolved methyl 7-(4-methyl-2-thienyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (420 mg), and to the mixture was added IN sodium hydroxide (8.4 ml). The mixture was stirred at room temperature for 15 hours. Under reduced pressure, the organic solvent was removed, and to the residue was added ethyl acetate. The mixture was extracted with water, and to the aqueous layer was added 6N hydrochloric acid to make the solution pH 4-5, which was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was removed to give 7-(4-methyl-2-thienyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (320 mg).

Aufarbeitung

  1. customUnder reduced pressure, the organic solvent was removed
  2. additionto the residue was added ethyl acetate
  3. extractionThe mixture was extracted with water
  4. additionto the aqueous layer was added 6N hydrochloric acid
  5. extractionwas extracted with ethyl acetate
  6. washwashed with saturated brine
  7. dry with materialdried with magnesium sulfate
  8. customUnder reduced pressure, the solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-1463498fd8184420a9c0d59892063a11
Quelldatensatz
uspto-grants-2002_07
Patentnummer
US06413947B1

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