Potassium Carbonate → HCID 57589084, Verbindung

HRID 1782756Notizen

Reaktionsgleichung

Br[CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:7][CH:6]=1.[CH:23]([C:25]1[CH:26]=[C:27]([CH:33]=[CH:34][C:35]=1[OH:36])[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:24].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH:23]([C:25]1[CH:26]=[C:27]([CH:33]=[CH:34][C:35]=1[O:36][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:7][CH:6]=1)[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:24]

Komponenten

Reaktionsbedingungen

Temperatur: 40 °C

Versuchsvorschrift

1.37 g (3.76 mmol) of 1-(3-bromopropyl)-4-(4-phenoxybutoxy)benzene, 0.79 g (3.76 mmol) of ethyl 3-formyl-4-hydroxybenzoate [CAS No. 82304-99-2] and 0.78 g (5.64 mmol) of potassium carbonate are dissolved in 20 ml of DMF, and the mixture is stirred at 40° C. for 16 hours. It is then concentrated, and the residue is taken up in 200 ml of water and extracted with dichloromethane (three times 100 ml). The combined organic phases are dried (sodium sulphate) and concentrated, and the crude product is purified by chromatography on silica gel (mobile phase gradient cyclohexane-->cyclohexane/ethyl acetate 5:1). 1.45 g of product are obtained.

Aufarbeitung

concentrationIt is then concentrated
extractionextracted with dichloromethane (three times 100 ml)
dry with materialThe combined organic phases are dried (sodium sulphate)
concentrationconcentrated
customthe crude product is purified by chromatography on silica gel (mobile phase gradient cyclohexane-->cyclohexane/ethyl acetate 5:1)

Quellen und Nachweise

ORD-Eintrag: ord-6ed629ecbb44458f9e3723db1e524f27
Quelldatensatz: uspto-grants-2009_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07498460B2

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