2-methyloctanoic acid

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: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: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: Then, 2.38 g (19.0 mmol) of thionyl chloride was maintained at a temperature of 36°~38° C. in a flask, to which was added dropwise 2.51 g (15.9 mmol) of the above (+)-2-methyl octanoic acid over 7 minutes with stirring. After the reaction with stirring at room temperature for 40 minutes, the reaction was further continued by stirring at a temperature of 80° C. for 30 minutes. Then, the reaction product was distilled to obtain 2.81 g (15.9 mmol, yield: 100%) of a colorless and transparent (+)-2-methyl octanoyl chloride. After the reaction with stirring at room temperature for 40 minutes by stirring at a temperature of 80° C. for 30 minutes Then, the reaction product was distilled

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

実験手順: Then, 2.02 g (12.8 mmol) of the above (+)-2-methyl octanoic acid, 2.02 g (11.9 mmol) of 4-hydroxy biphenyl and 10 ml of toluene were charged into a flask, and further 1.0 ml (13.7 mmol) of thionyl chloride was added with stirring, which were then reacted for 9 hours while maintaining at a temperature of 70°~80° C. After the completion of the reaction, the reaction mixture was cooled to room temperature, added with water to decompose excess thionyl chloride, washed with water and then dried on anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified through a column chromatography of silica gel to obtain 3.43 g of an oily (+)-biphenyl-2-methyloctanoate having a specific rotary power [α]25D =+16.3° (2.6% by weight, in chloroform). which were then reacted for 9 hours while maintaining at a temperature of 70°~80° C After the completion of the reaction washed with water dried on anhydrous magnesium sulfate After the solvent was distilled off the residue was purified through a column chromatography of silica gel

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

実験手順: To 21.2 g (147 mmol) of (-)-2-methyloctanol were added an aqueous solution of 330 ml of water and 46.4 g of concentrated sulfuric acid, which was stirred to form an emulsion. To this emulsion was added dropwise 63.4 g (401 mmol) of potassium permaganate over 7 hours. Then, the reaction mixture was added with 51.5 g of sodium bisulfite and poured into 270 ml of ice water together with 70 ml of ice water and 200 ml of ether. After the separation into two layers, the reaction product was extracted from the aqueous layer with ether, which was further extracted with a 10% aqueous solution of sodium hydroxide, added with ice and further with a concentrated hydrochloric acid to adjust the pH to not more than 1. Thereafter, the extraction with chloroform on the aqueous layer was performed, which was washed with water, dried on magnesium sulfate and filtered. The filtrate was concentrated and distilled under a reduced pressure to obtain 16.5 g (yield: 71%) of a colorless and transparent liquid of (+)-2-methyl octanoic acid. to form an emulsion After the separation into two layers the reaction product was extracted from the aqueous layer with ether, which was further extracted with a 10% aqueous solution of sodium hydroxide added with ice and further with a concentrated hydrochloric acid Thereafter, the extraction with chloroform on the aqueous layer which was washed with water dried on magnesium sulfate filtered The filtrate was concentrated distilled under a reduced pressure

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

実験手順: To 21.2 g (147 mmol) of (-)-2-methyloctanol were added an aqueous solution of 330 ml of water and 46.4 g of concentrated sulfuric acid, which was stirred to form an emulsion. To this emulsion was added dropwise 63.4 g (401 mmol) of potassium permaganate over 7 hours. Then, the reaction mixture was added with 51.5 g of sodium bisulfite and poured into 270 ml of ice water together with 70 ml of ice water and 200 ml of ether. After the separation into two layers, the reaction product was extracted from the aqueous layer with ether, which was further extracted with a 10% aqueous solution of sodium hydroxide, added with ice and further with a concentrated hydrochloric acid to adjust the pH to not more than 1. Thereafter, the extraction with chloroform on the aqueous layer was performed, which was washed with water, dried on magnesium sulfate and filtered. The filtrate was concentrated and distilled under a reduced pressure to obtain 16.5 g (yield: 71%) of a colorless and transparent liquid of (+)-2-methyl octanoic acid. to form an emulsion After the separation into two layers the reaction product was extracted from the aqueous layer with ether, which was further extracted with a 10% aqueous solution of sodium hydroxide added with ice and further with a concentrated hydrochloric acid Thereafter, the extraction with chloroform on the aqueous layer which was washed with water dried on magnesium sulfate filtered The filtrate was concentrated distilled under a reduced pressure

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

実験手順: Then, 2.38 g (19.0 mmol) of thionyl chloride was charged into a flask and maintained at a temperature of 36°~38° C., to which was added dropwise 2.15 g (15.9 mmol) of the above (+)-2-methyloctanoic acid in 7 minutes with stirring. The resulting mixture was stirred at room temperature for 40 minutes and at a temperature of 80° C. for 30 minutes. Then, the reaction product was distilled to obtain 2.81 g (15.9 mmol, yield 100%) of a colorless and transparent (+)-2-methyloctanoic acid chloride. maintained at a temperature of 36°~38° C., to which The resulting mixture was stirred at room temperature for 40 minutes and at a temperature of 80° C. for 30 minutes Then, the reaction product was distilled