反应详情

温度

-60 °C

420 ml of a 2M solution of the sodium salt of hexamethyldisilazane in THF are cooled to −60° C. under a nitrogen atmosphere, 350 ml of THF are added, then, dropwise, a solution of 57.6 g of 4-chlorophenylacetic acid in 70 ml of THF is added and the mixture is left stirring at −60° C. for one hour. 66 g of methyl 2,4-dichlorobenzoate are subsequently added dropwise at −60° C., the mixture is left stirring at −60° C. for 40 minutes and then the temperature is allowed to rise to 0° C. The reaction mixture is poured onto an ice/1 liter of 2N HCl mixture and extracted with ether, the organic phase is dried over Na2SO4, the solvent is concentrated under vacuum to a volume of 150 ml, 200 ml of pentane are added and the crystalline product formed is filtered off. 60 g of the expected compound are obtained.

1. waitthe mixture is left
2. waitthe mixture is left
3. stirringstirring at −60° C. for 40 minutes
4. customto rise to 0° C
5. extractionextracted with ether
6. dry with materialthe organic phase is dried over Na2SO4
7. concentrationthe solvent is concentrated under vacuum to a volume of 150 ml, 200 ml of pentane
8. additionare added
9. customthe crystalline product formed
10. filtrationis filtered off