乙酰氧基乙醛

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

实验步骤: The compound (500 mg, 2.17 mmol) obtained in Step 3 above was dissolved in dichloromethane (10 ml), 2-oxoethyl acetate (243 mg, 2.39 mmol) was added and the resulting mixture was stirred at room temperature for 1 hour. Then sodium triacetoxyborohydride (920 mg, 4.34 mmol) was added and the resulting mixture was stirred at room temperature for 3 hours. After reaction, saturated sodium bicarbonate solution (50 ml) was added and the resulting mixture was further stirred for 1 hour. The reaction mixture was diluted with dichloromethane and the organic layer was washed with brine. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue obtained was purified by silica gel column chromatography [chloroform:methanol=40:1→20:1 (v/v)] to give 544 mg (64%) of the title compound as a colorless oil. the resulting mixture was stirred at room temperature for 3 hours was added the resulting mixture was further stirred for 1 hour the organic layer was washed with brine The organic layer was dried over anhydrous sodium sulfate the solvent was evaporated under reduced pressure The residue obtained was purified by silica gel column chromatography [chloroform:methanol=40:1→20:1 (v/v)]

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

实验步骤: The compound (500 mg, 2.17 mmol) obtained in Step 3 above was dissolved in dichloromethane (10 ml), 2-oxoethyl acetate (243 mg, 2.39 mmol) was added and the resulting mixture was stirred at room temperature for 1 hour. Then sodium triacetoxyborohydride (920 mg, 4.34 mmol) was added and the resulting mixture was stirred at room temperature for 3 hours. After reaction, saturated sodium bicarbonate solution (50 ml) was added and the resulting mixture was further stirred for 1 hour. The reaction mixture was diluted with dichloromethane and the organic layer was washed with brine. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue obtained was purified by silica gel column chromatography [chloroform:methanol=40:1→20:1 (v/v)] to give 544 mg (64%) of the title compound as a colorless oil. the resulting mixture was stirred at room temperature for 3 hours was added the resulting mixture was further stirred for 1 hour the organic layer was washed with brine The organic layer was dried over anhydrous sodium sulfate the solvent was evaporated under reduced pressure The residue obtained was purified by silica gel column chromatography [chloroform:methanol=40:1→20:1 (v/v)]

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

实验步骤: To a mixture of 225 g of a 40% strength by weight aqueous solution of dimethylamine and 120 g of acetic acid was added with stirring and cooling, in the course of 15 min, a solution of 204 g of acetoxyacetaldehyde in 288 g (4 mol) of n-butyraldehyde, and the reaction mixture was subsequently stirred at 50° C. for 30 min. The reaction solutions were cooled down and the aqueous catalyst solution separated off to give, by fractional distillation, 169 g of 4-acetoxy-2-ethyl-2-butenal (b.p.=83°-93° C./6 mbar), corresponding to a yield of 54% of theory, based on acetoxyacetaldehyde, and 181 g of 2-ethyl-2-hexanal (b.p.=38°-70° C./20-60 mbar). was added cooling, in the course of 15 min The reaction solutions were cooled down the aqueous catalyst solution separated off

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

实验步骤: To a mixture of 225 g of a 40% strength by weight aqueous solution of dimethylamine and 120 g of acetic acid was added with stirring and cooling, in the course of 15 min, a solution of 204 g of acetoxyacetaldehyde in 288 g (4 mol) of n-butyraldehyde, and the reaction mixture was subsequently stirred at 50° C. for 30 min. The reaction solutions were cooled down and the aqueous catalyst solution separated off to give, by fractional distillation, 169 g of 4-acetoxy-2-ethyl-2-butenal (b.p.=83°-93° C./6 mbar), corresponding to a yield of 54% of theory, based on acetoxyacetaldehyde, and 181 g of 2-ethyl-2-hexanal (b.p.=38°-70° C./20-60 mbar). was added cooling, in the course of 15 min The reaction solutions were cooled down the aqueous catalyst solution separated off

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

实验步骤: The compound (500 mg, 2.17 mmol) obtained in Step 3 above was dissolved in dichloromethane (10 ml), 2-oxoethyl acetate (243 mg, 2.39 mmol) was added and the resulting mixture was stirred at room temperature for 1 hour. Then sodium triacetoxyborohydride (920 mg, 4.34 mmol) was added and the resulting mixture was stirred at room temperature for 3 hours. After reaction, saturated sodium bicarbonate solution (50 ml) was added and the resulting mixture was further stirred for 1 hour. The reaction mixture was diluted with dichloromethane and the organic layer was washed with brine. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue obtained was purified by silica gel column chromatography [chloroform:methanol=40:1→20:1 (v/v)] to give 544 mg (64%) of the title compound as a colorless oil. the resulting mixture was stirred at room temperature for 3 hours was added the resulting mixture was further stirred for 1 hour the organic layer was washed with brine The organic layer was dried over anhydrous sodium sulfate the solvent was evaporated under reduced pressure The residue obtained was purified by silica gel column chromatography [chloroform:methanol=40:1→20:1 (v/v)]