乙基 2-(2,4-二氯苯氧基)-2-甲基丙酸甲酯

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

实验步骤: A 5 N aqueous NaOH solution (0.83 ml) was added to a solution of 2-(2,4-dichloro-phenoxy)-2-methyl-propionic acid ethyl ester (383 mg, 1.38 mmol) in MeOH (6 ml) at room temperature. The mixture was stirred at room temperature for four hours, and 1 N HCl (4.5 ml) and H2O were then added, followed by extraction with AcOEt (×2). The organic layers were combined and sequentially washed with H2O and saturated brine, and then dried over Na2SO4 and concentrated under reduced pressure to give 2-(2,4-dichloro-phenoxy)-2-methyl-propionic acid (359 mg). followed by extraction with AcOEt (×2) sequentially washed with H2O and saturated brine dried over Na2SO4 concentrated under reduced pressure

反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2,4-Dichlorophenol (448 mg, 2.75 mmol) and K2CO3 (775 mg, 5.61 mmol) were continuously added to 2-bromo-2-methyl-propionic acid ethyl ester (800 mg, 4.10 mmol) in N,N-dimethylacetamide (4 ml) at room temperature. The mixture was stirred at 110° C. for 14 hours, and saturated NH4Cl and H2O were then added, followed by extraction with AcOEt (×2). The organic layers were combined and sequentially washed with H2O and saturated brine, and then dried over Na2SO4 and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane/AcOEt) to give 2-(2,4-dichloro-phenoxy)-2-methyl-propionic acid ethyl ester (389 mg, 50%). followed by extraction with AcOEt (×2) sequentially washed with H2O and saturated brine dried over Na2SO4 concentrated under reduced pressure The resulting residue was purified by silica gel column chromatography (n-hexane/AcOEt)

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

实验步骤: To a solution of KOH (2.48 g, 44.2 mmol, 15 eq) in H2O (12 mL) was added a solution of ethyl 2-(2,4-dichlorophenoxy)-2-methylpropionate (compound 5; 0.80 g, 2.89 mmol) in EtOH (12 mL). The solution was stirred at room temperature for 4 hours, then excess EtOH was removed under vacuum. The remaining aqueous solution was washed with EtOAc (10 mL), then acidified with concentrated aqueous HCl. The aqueous mixture was then extracted with EtOAc (10 mL), and the organic extract dried over Na2SO4, filtered, and evaporated to yield a thick, colorless oil which was used without further purification: 1H NMR (CDCl3) δ 7.42-7.41 (d, 1H), 7.19-7.15 (dd, 1H), 7.04-7.01 (d, 1H), 1.64 (s, 6H). excess EtOH was removed under vacuum The remaining aqueous solution was washed with EtOAc (10 mL) The aqueous mixture was then extracted with EtOAc (10 mL) the organic extract dried over Na2SO4 filtered evaporated to yield a thick, colorless oil which was used without further purification