反应详情

A mixture of the title compound from Example 302 Step A (2.44 g, 10.5 mmol), CCl3Br (8 mL) and Na2CO3 (480 mg, 4.5 mmol) in a sealed vessel was illuminated by a sunlamp for 30 h. Purification by silica gel flash chromatography using 8:1 to 6:1 to 4:1 hexanes:DCM as mobile phase yielded the title compound: 1H NMR (500 MHz, CD2Cl2) δ 8.03 (s, 1H), 7.92 (d, J=8.5 Hz, 1H), 7.65 (d, J=8.5 Hz, 1H).

1. customwas illuminated by a sunlamp for 30 h
2. customPurification by silica gel flash chromatography