反应详情

Pd(PPh3)4 (0.046 g, 0.4 mmol was added to a degassed solution of methyl (2,4-dibromothien-3-yl)acetate (2.51 g, 8 mmol) and 4-carboxybenzeneboronic acid (1.32 g, 8 mmol) in Na2CO3(40 mL, 0.4 M, 16 mmol) and CH3CN (40 mL). The mixture was heated to reflux overnight under argon for 16 h. The solution was filtered hot and the filtrate was concentrated to about half volume. The solution was extracted with CH2Cl2. The aqueous phase was acidified with concentrated HCl and the resulting solid was collected by vacuum filtration and washed with H2O to yield 4-(4-bromo-3-methoxycarbonylmethyl-thiophen-2-yl)-benzoic acid (1.98 g) which was used without further purification.

1. temperatureThe mixture was heated
2. temperatureto reflux overnight under argon for 16 h
3. filtrationThe solution was filtered hot
4. concentrationthe filtrate was concentrated to about half volume
5. extractionThe solution was extracted with CH2Cl2
6. filtrationthe resulting solid was collected by vacuum filtration
7. washwashed with H2O