Reaktion #11202
ord-66d5617ee3174b04900152f40608af0f
Reaktionsgleichung
Edukte
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1Sonstigeprepared
- 2Waschenchromatography was performed eluting with ethyl acetate/methanol/triethylamine (1:0:0 to 3:1:trace)
Vorschrift
Reaction of methyl ether (252) prepared as described in example 212 (80 mg, 0.15 mmol) according to The procedure described in example 80, except that the reaction was performed at 0° C. for 2 hours and chromatography was performed eluting with ethyl acetate/methanol/triethylamine (1:0:0 to 3:1:trace), gave amide (260) (65 mg, 83%) as a yellow/orange powder, mp 200–205° C. 1H NMR δ [(CD3)2SO] 11.00 (br s, 1H), 9.34 (s, 1H), 8.36 (d, J=2.4 Hz, 1H), 7.87 (br s, 1H), 7.66 (s, 1H), 7.54 (d, J=8.9 Hz, 1H), 7.44 (t, J=8.2 Hz, 1H), 7.18 (dd, J=8.2, 0.7 Hz, 1H), 7.12 (m, 2H), 4.64 (t, J=6.6 Hz, 2H), 3.68 (s, 3H), 3.05 (m, 2H), 2.56 (t, J=6.6 Hz, 2H), 2.23 (v br s, 2H), 2.15 (br s, 6H). Found: C, 58.98; H, 5.12; N, 9.59. C28H27ClN4O5.2H2O requires: C, 58.90; H, 5.47; N, 9.81.