反应详情

温度

100 °C

A mixture of 4-(4-bromo-benzyloxy)-2-hydroxy-benzoic acid (196.3 mg; 0.6075 mmol), 3-acetylbenzene boronic acid (99.7 mg; 0.6080 mmol) and Na2CO3 (−4 eq.) was dissolved in dimethoxymethane (4 mL) and H2O (2 mL). The solution was flushed with argon, Cl2Pd(PPh3)2 (˜2.5 mol %) was added and the mixture stirred under an atmosphere of argon at 100° C. for 16 hours. The resulting black solution was filtered (Gelman Acrodisc GHP, Ø25 mm) and slowly added to a cold 1 M HCl (aq.; 15 mL) solution. The precipitate was filtered off and thoroughly washed with water. Drying in vacuo yielded 195 mg (88%) of a greyish, solid compound with satisfactorily purity. Mp. 215-220° C. (decomposes); MS (ESI−): 361 (MH−)

1. customThe solution was flushed with argon, Cl2Pd(PPh3)2 (˜2.5 mol %)
2. additionwas added
3. filtrationThe resulting black solution was filtered (Gelman Acrodisc GHP, Ø25 mm)
4. additionslowly added to a cold 1 M HCl (aq.; 15 mL) solution
5. filtrationThe precipitate was filtered off
6. washthoroughly washed with water
7. customDrying in vacuo
8. customyielded 195 mg (88%) of a greyish, solid compound with satisfactorily purity