HCID 10892946, compound → HCID 11047916, compound

Participants

Reaction Steps

Iodide 6f (0.34 g; 1.0 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 CH3OH to afford 0.080 g (38%) of 1f as yellow prisms. mp>260 C; TLC (EtOAc): Rf=0.14; 1H NMR (DMSO-d6): δ 0.84 (t, 6H), 1.59 (m, 4H), 1.80 (br m, 8H), 2.80 (t, 4H), 3.55 (br m, 4H), 3.90 (br m, 4H); 13C NMR (DMSO-d6): δ 14.3, 23.4, 24.2, 26.9, 31.4, 46.8, 49.0, 132.9, 138.0, 163.7; UV/vis (CH3OH): max (M31 1cm−1)=287 (21200), 294 (20900), 309 (sh); LRMS (CI+): m/z (%): 208 (100), 413 (70) [M+H]+; HRMS (CI+): calcd for C22H33N6O2 413.2665; found 413.2662; Anal. calcd for C22H32N6O20.33(H2O): C, 63.13; H, 7.87; N, 20.08; found: C, 63.21; H, 7.82; N, 20.08.

Provenance & Evidence