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Hydrochloric Acid → HCID 14722395, Verbindung

HRID 1031682
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1031682
[C:1](OC(=O)C)(=[O:3])[CH3:2].[OH:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12].[C:35]([O-])(=O)[CH3:36].[Na+].Cl>O.C(OCC)(=O)C>[C:1]([N:23]([C:21]1[C:20]([O:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[CH:19][C:10]2[C:11](=[O:12])[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:35]([CH3:36])[O:8][C:9]=2[CH:22]=1)[S:24]([CH3:27])(=[O:26])=[O:25])(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 10620577HCID 10620577, Verbindung

Produkt 1

HCID 14722395HCID 14722395, VerbindungAusbeute 55,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

2.55 ml of acetic anhydride was added to 850 mg of ethyl 2-(2-hydroxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate and 540 mg of sodium acetate. The mixture was stirred for 10 minutes at 110°-120° C. The reaction mixture was introduced into a mixture of 20 ml of ethyl acetate and 20 ml of water. The resulting mixture was adjusted to pH 2 with 2N hydrochloric acid. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: a 5 : 1 mixture of toluene and ethyl acetate) to obtain 550 mg (yield: 55.6%) of 7-(N-acetyl-N-methylsulfonylamino)-3-ethoxycarbonyl-2-methyl-6-phenoxy-4H-1-benzopyran-4-one.

Aufarbeitung

  1. customThe organic layer was separated
  2. washwashed with water
  3. dry with materiala saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by a column chromatography (eluant
  6. additiona 5 : 1 mixture of toluene and ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-a431ed6f23544814a75aebda73c6481c
Quelldatensatz
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04954518

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