反应详情

温度

130 °C

4-Chloro-2-methoxy-1-nitrobenzene (4.84 g, 25.8 mmol) and diethyl phosphonate (3.92 g, 28.4 mmol) were added in a 250 mL round-bottomed flask. DMF (100 mL) was added to give a yellow solution. Potassium phosphate (6.02 g, 28.4 mmol) and palladium (II) acetate (0.290 g, 1.29 mmol) were added. Nitrogen was bubbled through the solution for 20 min before xantphos (1.045 g, 1.81 mmol) was added. The reaction was heated to 130° C. and stirred at that temperature for 4 h. After it was cooled to RT, the solution was concentrated in vacuo to remove the solvent, and to the residue was added water (60 mL) and DCM (40 mL). After partition, the aqueous layer was washed with DCM (2×20 mL). The aqueous layer was acidified using 12 N HCl (10 mL), and DCM was added (50 mL). After partition and extraction with DCM (2×30 mL), the DCM solution was combined and concentrated to give the product without further purification (2.4 g, 36% yield).

1. customto give a yellow solution
2. additionwas added
3. temperatureAfter it was cooled to RT
4. concentrationthe solution was concentrated in vacuo
5. customto remove the solvent
6. additionto the residue was added water (60 mL) and DCM (40 mL)
7. customAfter partition
8. washthe aqueous layer was washed with DCM (2×20 mL)
9. additionwas added (50 mL)
10. customAfter partition
11. extractionextraction with DCM (2×30 mL)
12. concentrationconcentrated
13. customto give the product
14. customwithout further purification (2.4 g, 36% yield)