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Sulfuric Acid → HCID 15295001, Verbindung

HRID 327944
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 327944
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:18]=[CH:17][C:11]2[C:12](=[O:16])[CH2:13][CH2:14][O:15][C:10]=2[C:9]=1[CH2:19][CH2:20][CH3:21].C([O:24][C:25]([C:27]1[O:28][C:29]2[C:35]([OH:36])=[CH:34][CH:33]=[CH:32][C:30]=2[CH:31]=1)=[O:26])C.C(=O)([O-])[O-].[K+].[K+].O.[OH-].[Li+].S(=O)(=O)(O)O>C1COCC1.O.C(OCC)(=O)C.CCOCC.CC(=O)CC>[O:16]=[C:12]1[C:11]2[CH:17]=[CH:18][C:8]([O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][O:36][C:35]3[C:29]4[O:28][C:27]([C:25]([OH:26])=[O:24])=[CH:31][C:30]=4[CH:32]=[CH:33][CH:34]=3)=[C:9]([CH2:19][CH2:20][CH3:21])[C:10]=2[O:15][CH2:14][CH2:13]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 5

HCID 1118Sulfuric AcidHCID 11430Potassium CarbonateHCID 168937Lithium hydroxide, monohydrateHCID 19921918HCID 19921918, VerbindungHCID 21400703Ethyl 7-hydroxy-1-benzofuran-2-carboxylate

Produkt 1

HCID 15295001HCID 15295001, Verbindung
Ausbeute 74,9 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 6569Methyl Ethyl KetoneLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of 0.556 g (1.57 mmol) of 7-[(5-bromopentyl)oxy]-2,3-dihydro-8-propyl-4H-1-benzopyran-4-one, 0.323 g (1.57 mmol) of 7-hydroxy-2-benzofurancarboxylic acid ethyl ester, 0.866 g (6.26 mmol) of anhydrous granular potassium carbonate and 16 mL of 2-butanone was stirred and refluxed for 16.5 hrs. The resulting slurry was filtered with suction and the solids were washed thoroughly with ethyl acetate. The filtrate and washes were combined and concentrated in vacuo and the residue was purified by flash chromatography on 70 g of silica gel, eluting with 4:1 hexane-ethyl acetate giving 0.527 g (70%) of 7-[5-[(3,4-dihydro-4-oxo-8-propyl-2H-1-benzopyran-7-yl)oxy]pentyloxy]benzenepropanoic acid ethyl ester as a white solid, mp 79.5°-81° C. A mixture of 0.262 g (0.55 mmol) of this ester in 3.5 mL of THF and 3.5 mL of water was treated with 35.1 mg (0.84 mmol) of lithium hydroxide monohydrate and the mixture was stirred for 17.5 hr. After being acidified with 16 mL of 3N aqueous sulfuric acid, the resulting mixture was worked-up with ether and ethyl acetate in the usual manner. The crude product was recrystallized from hexane-ethyl acetate to give 0.185 g (74.9%) of the title compound as a white solid, mp 152°-153.5° C.

Aufarbeitung

  1. temperaturerefluxed for 16.5 hrs
  2. filtrationThe resulting slurry was filtered with suction
  3. washthe solids were washed thoroughly with ethyl acetate
  4. concentrationconcentrated in vacuo
  5. customthe residue was purified by flash chromatography on 70 g of silica gel
  6. washeluting with 4:1 hexane-ethyl acetate giving 0.527 g (70%) of 7-[5-[(3,4-dihydro-4-oxo-8-propyl-2H-1-benzopyran-7-yl)oxy]pentyloxy]benzenepropanoic acid ethyl ester as a white solid, mp 79.5°-81° C
  7. stirringthe mixture was stirred for 17.5 hr
  8. customThe crude product was recrystallized from hexane-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-9d69c55117a2426da35c84b996250309
Quelldatensatz
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05273999

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