反应详情

温度

125 °C

A mixture of 5B (60 mg, 0.14 mmol), N-(5-amino-2-methylphenyl)acetamide (46.8 mg, 0.29 mmol), Pd2(dba)3 (13.1 mg, 0.014 mmol), Xantphos (18.2 mg, 0.031 mmol), copper(I) iodide (13.6 mg, 0.071 mmol) and Cs2CO3 (186 mg, 0.57 mmol) in DMA (1 mL) was purged with nitrogen and heated at 125° C. After 1.5 hours, the reaction mixture was diluted with ethyl acetate, washed with 15% NH4OH, dried over Na2SO4, and concentrated to dryness under reduced pressure. The resulting oil was purified by silica column chromatography (gradient=0%-100% hexanes to ethyl acetate in 12 min.) to isolate 5C (47.5 mg, 60.7% yield). HPLC: Rt=3.805 min (YMC S5 ODS 4.6×50 mm, 10-90% aqueous methanol containing 0.2% H3PO4, 4 min gradient, monitored at 220 nm). MS (ES): m/z=549.2 [M+H]+.

1. customwas purged with nitrogen
2. additionthe reaction mixture was diluted with ethyl acetate
3. washwashed with 15% NH4OH
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness under reduced pressure
6. customThe resulting oil was purified by silica column chromatography (gradient=0%-100% hexanes to ethyl acetate in 12 min.)