Toluene → HCID 11576813, compound

Participants

Reaction Steps

(2,2-Diethoxyethyl)-{6-[4-(2-dimethylamino-ethoxy)-phenyl]-5-phenyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl}-amine (Example 33, Step C; 50 mg, 0.12 mmol) was combined with 12 μl ethanedithiol in 5 ml toluene, then the mixture was heated to reflux for 4 h. After that time the mixture was cooled to rt, concentrated and purified by chromatography on silica gel (CH2Cl2:MeOH=95:5) to give the title compound. 1H-NMR (400 MHz, DMSO-d6) δ 2.21 (s, 6H), 2.61 (t, 2H, J=5.73 Hz), 3.16-3.05 (m, 4H), 3.61 (t, 2H, J=6.07 Hz), 4.03 (t, 2H, J=5.77 Hz), 4.68 (t, 1H, J=6.29 Hz), 5.23 (t, 1H, J=5.86 Hz), 6.86 (d, 2H, J=8.84 Hz), 7.25 (d, 2H, J=8.80 Hz), 8.14-7.38 (m, 5H), 8.21 (s, 1H), 12.12 (s, 1H). Mass Spectrum (ESI) m/e=492 (M+1).

Provenance & Evidence