methyl 3-(2-chlorophenyl)-3-oxopropanoate

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which

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

実験手順: A mixture of methyl 2-chlorobenzoylacetate (Acros; 266 mg, 1.25 mmol) and N,N-dimethylformamide dimethylacetal (161 mg, 1.35 mmol) was stirred at rt under N2 for 2 weeks. The reaction was then concentrated in vacuo and the residue was adsorbed on silica gel and chromatographed. Elution with 3:1 EtOAc/hexanes afforded 193 mg of the title compound as a yellow solid. The reaction was then concentrated in vacuo chromatographed Elution with 3:1 EtOAc/hexanes

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a flask containing 3-(2-chlorophenyl)-3-oxo-propionic acid, methyl ester (20 g, 94 mmol) was added triethylorthoformate (37.5 mL, 225.6 mmol) and acetic anhydride (63 mL, 667 mmol). The resulting mixture was heated to 130° C. with stirring for a total of 2 hours, then stirred over night at room temperature. The reaction mixture was concentrated under reduced pressure to provide a crude oil, which was used directly in the next step. stirred over night at room temperature The reaction mixture was concentrated under reduced pressure to provide a crude oil, which