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With sodium acetate; In N,N-dimethyl-formamide; |
EXAMPLE 1A 2-Acetyloxy-1-(2,4-difluorophenyl)ethanone 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 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 Na2 SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluding with CH2 Cl-2-hexane to obtain 198 g of the title compound. STR103 |
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With sodium acetate; In N,N-dimethyl-formamide; |
EXAMPLE 1a 2-Acetyloxy-1-(2,4-difluorophenyl)ethanone 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 Na2 SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluding with CH2 Cl-2-hexane to obtain 198 g of the title compound. STR106 |
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With sodium acetate; In N,N-dimethyl-formamide; |
Example 1a 2-Acetyloxy-1-(2,4-difluorophenyl)ethanone 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 Na2 SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluding with CH2 Cl-2-hexane to obtain 198 g of the title compound. STR101 |
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With sodium acetate; In acetic acid; |
(i) 2-Acetoxy-2',4'-difluoroacetophenone 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 (Na2 SO4). 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. |
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With sodium acetate; In N,N-dimethyl-formamide; |
EXAMPLE 1a 2-Acetyloxy-1-(2,4-difluorophenyl)ethanone 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 20C 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, eluding with CH2Cl2-hexane to obtain 198 g of the title compound. |
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