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, High Resolution Electro-Spray Ionisation Mass Spectra (HR-ESI-MS) were obtained from the 'Centre Régional de Mesures Physiques de l
, General procedure for the synthesis of compound 1
, at various temperature were added anhydrous pyridine (1 eq) then SOCl2. The reaction mixture was stirred till consuming of starting material, then water and ethyl acetate were added. Layers were separated and organic layer was washed with 1N HCl. Organic layer was dried over MgSO4
, 171-172°C . 1 H NMR (400 MHz, CDCl3) ? 7.19 (d, 1H, J = 10.0 Hz
,
,
, 39 (s, 3H, H-19), 1.26 -1.12 (m, 1H, H-7), 0.88 (s, 3H, H-18), H-8), 1.48 (m, 1H ,H-14), vol.1
, H-21), 4.84 (d, J = 17.5 Hz, 1H, H-21), 2.98 -2.83 (m, 1H, OH), 2.73 (m, 1H, H-16), 2.69 -2.59 (m, 2H, H-6 + H-12), 2.44 -2.35 (m, 1H, H-6), 2.34 -2.24 (m, 1H, 220-222°C. 1 H NMR (400 MHz, CDCl3) ? 7.19 (d, J = 10.0 Hz, 1H, H-1), 6.25 (dd, J = 10.0, 1.9 Hz, 1H, H-2), 6.03 (m, 1H, H-4), 5.55 (m, 1H, H-11), 5.03 (d, J = 17.5 Hz, vol.1
, C-6 or C-12), 32.3 (C-6 or C-12), 14.5 (C-18). EI-MS (M+H) : m, vol.35, pp.20-28
, 54-56°C. 1 H NMR (400 MHz, CDCl3) ? 7.10 (d, J = 10.0 Hz, 1H, H-1), vol.6
, 08 (s, 3H, H-23), 1.77 (m, 1H, H-16), vol.2
, MHz, CDCl3) ? 205.7 (C-20), vol.186, pp.140-147
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