反应详情

温度

60 °C

A mixture of 4-(3-iodo-phenyl)-8-pyrrol-1-yl-1,3-dihydro-benzo[b][1,4]diazepin-2-one (Example 7) (214 mg, 0.5 mmol), Pd(OAc)2 (4 mg, 3 mol %), PPh3 (8mg, 8 mol %) and HDMS (0.52 mL, 2.5 mmol) in DMF (2 mL) was stirred under CO atmosphere at 60° C. for 4 h. The mixture was taken up in EtOAc, washed with 1 N HCl, sat. NaHCO3-sol. and brine, dried over MgSO4. Removal of the solvent in vacuum left a dark brown solid, which was purified by silica gel column chromatography with EtOAc/MeOH 95:5. Obtained as a yellow-brown solid (97 mg).

1. washwashed with 1 N HCl, sat. NaHCO3-sol
2. dry with materialand brine, dried over MgSO4
3. customRemoval of the solvent in vacuum
4. waitleft a dark brown solid, which
5. customwas purified by silica gel column chromatography with EtOAc/MeOH 95:5