[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]=1Potassium 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.
読み込み中…
