(3R)-3-methylheptanoic acid

反应条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: At room temperature, 60 g of [(R)-1-methylpentyl]-malonic acid (0.318 mol) were dissolved in 120 ml of xylene in a three-neck flask with internal thermometer, condenser and stirrer. The mixture was heated to 125° C. for 5 h. After cooling to 25° C., the mixture was admixed with 200 ml of 2N sodium hydroxide solution. After phase separation, the aqueous phase was admixed with 200 ml of ether and, with cooling, with 180 ml of 15% by weight hydrochloric acid. After phase separation, the aqueous phase was extracted twice with 100 ml of ether. The combined organic phases were washed with 50 ml of water and then dried over sodium sulfate. After solvent had been distilled off, (R)-3-methylheptanoic acid was distilled and obtained in a yield of 35.5 g (77% of theory) with >99% ee and >99% chemical purity (b.p.: 67-68° C. at 0.45 mbar). After cooling to 25° C. After phase separation with cooling, with 180 ml of 15% by weight hydrochloric acid After phase separation the aqueous phase was extracted twice with 100 ml of ether The combined organic phases were washed with 50 ml of water dried over sodium sulfate After solvent had been distilled off (R)-3-methylheptanoic acid was distilled obtained in a yield of 35.5 g (77% of theory) with >99% ee and >99% chemical purity (b.p.: 67-68° C. at 0.45 mbar)

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

实验步骤: In a 500 ml flask were charged 300 ml of methanol, 35.5 g of (R)-3-methylheptanoic acid obtained in Step 3, and 0.5 g of concentrated sulfuric acid, and the mixture was heated at a methanol refluxing temperature for 18 hours. Methanol was distilled off under reduced pressure, and the residue was extracted with diethyl ether. The extract was washed with water, neutralized with a sodium carbonate aqueous solution, and then washed with a sodium chloride aqueous solution. Diethyl ether was removed by distillation, and the residue was distilled under reduced pressure to obtain 29 g (76.8%) of the titled compound (b.p.: 80° C./20 mmHg). Methanol was distilled off under reduced pressure the residue was extracted with diethyl ether The extract was washed with water washed with a sodium chloride aqueous solution Diethyl ether was removed by distillation the residue was distilled under reduced pressure

反应条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: At room temperature, 60 g of [(R)-1-methylpentyl]-malonic acid (0.318 mol) were dissolved in 120 ml of xylene in a three-neck flask with internal thermometer, condenser and stirrer. The mixture was heated to 125° C. for 5 h. After cooling to 25° C., the mixture was admixed with 200 ml of 2N sodium hydroxide solution. After phase separation, the aqueous phase was admixed with 200 ml of ether and, with cooling, with 180 ml of 15% by weight hydrochloric acid. After phase separation, the aqueous phase was extracted twice with 100 ml of ether. The combined organic phases were washed with 50 ml of water and then dried over sodium sulfate. After solvent had been distilled off, (R)-3-methylheptanoic acid was distilled and obtained in a yield of 35.5 g (77% of theory) with >99% ee and >99% chemical purity (b.p.: 67-68° C. at 0.45 mbar). After cooling to 25° C. After phase separation with cooling, with 180 ml of 15% by weight hydrochloric acid After phase separation the aqueous phase was extracted twice with 100 ml of ether The combined organic phases were washed with 50 ml of water dried over sodium sulfate After solvent had been distilled off (R)-3-methylheptanoic acid was distilled obtained in a yield of 35.5 g (77% of theory) with >99% ee and >99% chemical purity (b.p.: 67-68° C. at 0.45 mbar)