反应详情

Compound 5 (1.0 g, 4.0 mmol, 1.0 eq), tert-Butyl carbamate (560 mg, 4.78 mmol, 1.20 eq), tris(dibenzylideneacetone) dipalladium-chloroform adduct (120 mg, 0.116 mmol, 0.0300 eq), sodium tert-butoxide (530 mg, 5.52 mmol, 1.40 eq), and 2-Di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (180 mg, 0.424 mmol, 0.0900 eq) stirred in toluene (15 mL) at rt overnight. The mixture was filtered through celite and washed with 5% MeOH in CH2Cl2. The filtrate was collected and concentrated in vacuo to afford 1.1 g (100%) of the title compound as an orange solid: 1H NMR (400 MHz, DMSO-d6) δ 9.79 (s, 1H), 9.05 (s, 1H), 8.72 (s, 2H), 8.45 (d, J=1.7 Hz, 1H), 8.10 (t, J=2.5 Hz, 1H), 7.69 (s, 1H), 1.45 (s, 9H); ES-MS [M+1]+: 289.1.

1. filtrationThe mixture was filtered through celite
2. washwashed with 5% MeOH in CH2Cl2
3. customThe filtrate was collected
4. concentrationconcentrated in vacuo