Water → 4-(3-Fluoropropoxy)benzaldehyde

HRID 217554

Reaktionsgleichung

[F-:1].[K+].C1N2CCOCCOCCN(CCOCCOCC2)CCOCCOC1.[CH:29]([C:31]1[CH:45]=[CH:44][C:34]([O:35][CH2:36][CH2:37][CH2:38]OS(C)(=O)=O)=[CH:33][CH:32]=1)=[O:30].O>C(#N)C>[F:1][CH2:38][CH2:37][CH2:36][O:35][C:34]1[CH:44]=[CH:45][C:31]([CH:29]=[O:30])=[CH:32][CH:33]=1

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

Potassium fluoride (Fluka, 7.2 mg, 0.124 mmol) and kryptofix 222 (Fluka, 46.7 mg, 0.124 mmol) were dissolved in dry acetonitrile (2.5 ml). After 10 min the mixture was added to a stirred solution of methanesulfonic acid 3-(4-formylphenoxy)propyl ester 13 (16.0 mg, 0.062 mmol) in dry acetonitrile (1.5 ml). The reaction mixture was heated at 60° C. for 30 minutes. The product was confirmed by analytical HPLC (column Phenomenex Luna C18(2) 3 μm 4.6×50 mm, solvents: A=water/0.1% TFA and B=acetonitrile/0.1% TFA; gradient 10-80% B over 10 min; flow 2.0 ml/min, UV detection at 214 and 254 nm) co-eluting with commercial standard (Fluorochem) at 5.0 minutes.

Aufarbeitung

customat 5.0 minutes

Quellen und Nachweise

ORD-Eintrag: ord-6799a10eada64d6688f75700a3445624
Quelldatensatz: uspto-grants-2012_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08197793B2

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