HCID 10894751, compound → HCID 11731371, compound

Participants

Reaction Steps

Iodide 6b (0.44 g; 1.1 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 CHCl3. Slow addition of CH3CN caused a brown solid to precipitate. This material was collected by filtration and washed with CH3CN to afford 0.12 g (40%) of 1b as an off-white solid. mp 173–174 C; TLC (CH2Cl2-EtOAc, 1:1): Rf=0.51; 1H NMR (DMSO-d6): δ 0.85 (t, 6H), 1.60 (m, 4H), 2.90 (t, 4H), 4.42 (d, 4H), 6.99 (d, 411), 7.05 (t, 2H), 8.20 (br t, 2H); 13C NMR (DMSO-d6): δ 14.1, 23.1, 30.2, 41.8, 110.9, 131.0, 141.7, 145.5, 161.3, 163.8, 164.7; UV/vis (CH3OH): max (M−1cm−1)=287 (21800), 294 (20700), 309 (10700); LRMS (CI+): m/z (%): 557 (100) [M+H]+; HRMS (CI+): calcd for C28H29F4 N6O2 557.2288; found 557.2292.

Provenance & Evidence