反应详情

16.5 g (0.55 mol) of sodium hydride (80%) are stirred in 500 ml of tetrahydrofuran and 123.3 g (0.55 mol) of phosphonoacetic acid triethyl ester are added dropwise to give a clear solution. Then over 15 minutes a solution of 83.1 g (0.50 mol) of 3,4-dimethoxybenzaldehyde in 200 ml of tetrahydrofuran are added. The mixture is then stirred under reflux for 30 minutes. After cooling, the clear solution is separated from the insoluble material which is dissolved in 500 ml of water and extracted twice with 250 ml of toluene. The tetrahydrofuran solution is evaporated to dryness and the residue is dissolved in the toluene extract. This solution is washed three times with water, dried and the solvent evaporated.

1. customto give a clear solution
2. temperatureunder reflux for 30 minutes
3. temperatureAfter cooling
4. customthe clear solution is separated from the insoluble material which
5. dissolutionis dissolved in 500 ml of water
6. extractionextracted twice with 250 ml of toluene
7. customThe tetrahydrofuran solution is evaporated to dryness
8. dissolutionthe residue is dissolved in the toluene
9. extractionextract
10. washThis solution is washed three times with water
11. customdried
12. customthe solvent evaporated