HCID 11068117, compound → HCID 10874022, compound

Participants

Reaction Steps

Iodide 6e (0.55 g; 1.6 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 recrystallized from EtOAc to afford 0.13 g (33%) of 1e as colorless prisms. mp>260 C; TLC (EtOAc): Rf=0.31; 1H NMR (CDCl3): δ 0.91 (t, 6H), 1.65 (m, 4H), 1.82 (m, 44), 3.00 (t, 4H), 3.34 (s, 6H), 3.48 (m, 8H), 7.29 (br t, 2H); 13C NMR (DMSO-d6): δ 14.3, 24.1, 26.7, 32.3, 61.9, 72.3, 137.5, 145.1, 167.3; UV/vis (CH3OH): max (M−1cm−1)=287 (25600), 295 (25400), 309 (13800); LRMS (CI+): m/z (%): 449 (100) [M+H]+; HRMS (CI+): calcd for C22H37N6O4 449.2876; found 449.2875; Anal. calcd for C22H36N6O4: C, 58.91; H, 8.09; N, 18.74; found: C, 59.00; H, 8.09; N, 18.78.

Provenance & Evidence