[2-(2,4-difluorophenyl)-2-oxoethyl] acetate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of Nal, and 3 L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1 L. Pour the residue into 6 L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR101## then concentrate it to 1 L Pour the residue into 6 L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of NaI, and 3L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1L. Pour the residue into 6L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR100## then concentrate it to 1L Pour the residue into 6L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of NaI, and 3L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1L. Pour the residue into 6L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR100## then concentrate it to 1L Pour the residue into 6L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-chloro-2',4'-difluoroacetophenone (19.0 g) and anhydrous sodium acetate (16.4 g) in acetic acid (50 ml) was heated under reflux for 4 hours and then evaporated. The residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with sodium bicarbonate solution and dried (Na2SO4). Evaporation of the solvent gave an oil which was triturated with hexane. The resulting solid was filtered off, washed with hexane and dried to give the title compound, (16.2 g), m.p. 54°-56°. under reflux for 4 hours evaporated The residue was partitioned between ethyl acetate and water The organic layer was separated washed with sodium bicarbonate solution dried (Na2SO4) Evaporation of the solvent gave an oil which was triturated with hexane The resulting solid was filtered off washed with hexane dried

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of Nal, and 3 L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1 L. Pour the residue into 6 L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR94## then concentrate it to 1 L Pour the residue into 6 L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of Nal, and 3 L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1 L. Pour the residue into 6 L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR94## then concentrate it to 1 L Pour the residue into 6 L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of Nal, and 3 L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1 L. Pour the residue into 6 L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR94## then concentrate it to 1 L Pour the residue into 6 L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of Nal, and 3 L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1 L. Pour the residue into 6 L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR106## then concentrate it to 1 L Pour the residue into 6 L of cold dilute aqueous HCl extract with EtOAc Wash the extract with brine dry it over anhydrous Na2SO4 filter the so-formed mixture evaporate the filtrate to leave a residue Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane