反应详情

温度

100 °C

A 10 mL flask was charged with 4-chloro-2-(2,5,6-trichloro-pyrimidin-4-yl)-phenol (75 mg, 0.24 mmol) and N-methylpyrrolidinone (3.0 mL) under a N2 atmosphere. The solution was purged with N2 for, 10 min. Copper (I) thiophene-2-carboxylate (60 mg, 0.32 mmol, 1.3 equiv.) was added and the mixture was heated to 100° C. for 2 h. The reaction mixture was cooled to rt and added to aq. HCl (0.1 M, 6.0 mL) slowly and stirred for 15 min. Additional aq. HCl (0.1 M, 3.0 mL) was added and the mixture was stirred for 20 min. The resulting solid was collected by filtration, rinsed with water, and dried to give a tan solid (55 mg, 83%). GC-MS (CI): mass calcd. for C10H3Cl3N2O, 271.9; m/z found, 272.0. 1H NMR (CDCl3): 8.22 (d, J=2.1 Hz, 1H), 7.75 (dd, J=8.9, 2.1 Hz, 1H), 7.69 (d, J=9.0 Hz, 1H).

1. customThe solution was purged with N2 for, 10 min
2. temperatureThe reaction mixture was cooled to rt
3. stirringthe mixture was stirred for 20 min
4. filtrationThe resulting solid was collected by filtration
5. washrinsed with water
6. customdried