1-(4-氯苯基)-2-(2,4-二氯苯基)乙酮

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 411 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, followed dropwise by a solution of 67.7 g of 2,4-dichlorophenylacetic acid in 70 ml of THF and the mixture is kept stirred for 2 hours while the temperature is maintained below −40° C. 53.5 g of methyl 4-chlorobenzoate are then added dropwise and at −60° C. and the mixture is kept stirred while the temperature is allowed to rise to 10° C. The reaction mixture is poured over an ice/1 liter 2N HCl mixture, the organic phase is washed with a saturated NaHCO3 solution, with water, extracted with ether, the organic phase is dried over Na2SO4 and the solvent is evaporated under vacuum. The residue is taken up in pentane and the crystallized product formed is drained. 70 g of the expected compound are obtained. is maintained below −40° C the mixture is kept stirred while the temperature to rise to 10° C the organic phase is washed with a saturated NaHCO3 solution, with water extracted with ether the organic phase is dried over Na2SO4 the solvent is evaporated under vacuum the crystallized product formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 411 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, followed dropwise by a solution of 67.7 g of 2,4-dichlorophenylacetic acid in 70 ml of THF and the mixture is kept stirred for 2 hours while the temperature is maintained below −40° C. 53.5 g of methyl 4-chlorobenzoate are then added dropwise and at −60° C. and the mixture is kept stirred while the temperature is allowed to rise to 10° C. The reaction mixture is poured over an ice/1 liter 2N HCl mixture, the organic phase is washed with a saturated NaHCO3 solution, with water, extracted with ether, the organic phase is dried over Na2SO4 and the solvent is evaporated under vacuum. The residue is taken up in pentane and the crystallized product formed is drained. 70 g of the expected compound are obtained. is maintained below −40° C the mixture is kept stirred while the temperature to rise to 10° C the organic phase is washed with a saturated NaHCO3 solution, with water extracted with ether the organic phase is dried over Na2SO4 the solvent is evaporated under vacuum the crystallized product formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.5 ml of bromine are added dropwise to a solution of 1-(4-chlorophenyl)-2-(2,4-dichlorophenyl)ethanone in dichloromethane (200 ml). The mixture is stirred for 4 hours at room temperature. The reaction medium is washed with water, with saturated aqueous NaHCO3 solution and then with aqueous NH4Cl solution. The organic phase is dried over Na2SO4, filtered and evaporated to dryness. The expected product is precipitated from pentane (yield=94%). The reaction medium is washed with water, with saturated aqueous NaHCO3 solution The organic phase is dried over Na2SO4 filtered evaporated to dryness

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 32 g of LiHMDS are placed in 245 ml of THF at 0° C., and 40 g of (4-chlorophenyl) ((trimethylsilyl)oxy)acetonitrile are added slowly at −78° C., followed by 32.64 g of 2,4-dichloro-1-(chloromethyl)benzene. The temperature is allowed to return to AT overnight, and the reaction is then hydrolyzed with 170 ml of a 3N HCl solution, with gases being trapped in a solution of KOH (4N). After separation by settling out, the organic phase is evaporated, then taken up in DCM and agitated for 1 hour with 170 ml of NaOH (2N). The DCM is evaporated off and the expected compound is then crystallized from pentane. 38.6 g are obtained, Mp=119° C. to return to AT overnight After separation the organic phase is evaporated The DCM is evaporated off the expected compound is then crystallized from pentane 38.6 g are obtained