HCID 10870074, compound → HCID 11759373, compound

Participants

Reaction Steps

Iodide 6a (0.35 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 dissolved in CH2Cl2. Upon standing, a white solid precipitated. This material was collected by filtration and was washed with ice-cold CH2Cl2 to afford 0.080 g (43%) of 1a. mp>260 ÿC; TLC (EtOAc): Rf=0.32; 1H NMR (DMSO-d6): δ 0.83 (t, 6H), 1.61 (m, 4H), 2.73 (d, 6H), 2.89 (t, 4H), 7.50 (br t, 2H); 13C NMR (DMSO-d6): δ 13.1, 21.9, 24.7, 30.2, 130.3, 135.6, 163.0; UV/vis (CH3OH): λmax (ε M−1cm−1)=286 (18500), 294 (18200), 309 (9860); Anal. calcd for C16H24N6O2.0.25(CH2Cl2): C, 55.19; H, 6.98; N, 23.76; found: C, 54.93; H, 6.71; N, 23.74.

Provenance & Evidence