HCID 11111754, compound → HCID 10984079, compound

Participants

Reaction Steps

Iodide 6c (0.45 g; 1.2 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was triturated with CH3CN. The solid that remained undissolved was collected by filtration and washed with CH3CN to afford 0.30 g (38%) of 1c as an off-white microcrystalline solid. An analytical sample was recrystallized from CH3OH. mp 226–227 C; TLC (CH2Cl2-EtOAc, 1:1): Rf=0.60; 1H NMR (CD2Cl2): δ 0.80 (t, 6H), 1.59 (m, 4H), 2.21 (s, 6H), 2.86 (t, 4H), 4.39 (d, 4H), 7.05 (dd, 8H), 7.22 (br t, 2H); 13C NMR (DMSO-d6): δ 14.2, 21.4, 23.3, 27.0, 49.6, 128.3, 129.9, 131.0, 137.0, 138.7, 164.2; UV/vis (CH3OH): max (M−1cm−1)=287 (25100), 295 (25100), 310 (13700); LRMS (CI+): m/z (%): 513 (100) [M+H]+; HRMS (CI+): calcd for C30H37N6O2 513.2978; found 513.2981; Anal. calcd for C30H36N6O20.33(H2O): C, 68.68; H, 7.17; N, 16.02; found: C, 68.58; H, 7.17; N, 16,11.

Provenance & Evidence