Hydrochloric Acid → alpha-Oxocyclohexaneacetic acid

温度

60 °C

To a solution of ethyl cyclohexyloxoacetate (46 g) in MeOH (25 mL) was added water (60 mL) and NaOH (50% 20 mL) at 0-15° C. The reaction mixture was heated to 60° C. for 1.5 h. The reaction mixture was cooled with ice-water bath, and acidified with 15% HCl till pH 1. The mixture was extracted with ethyl acetate (2×250 mL). The extracts were washed with brine, dried with sodium sulfate. The drying agent was removed by filtration and the solvent was removed to give a low melting solid (39 g, 99%). 1H NMR: δ 1.15-1.40 (m, 5H,), 1.62-1.96 (m, 5H). 3.20 (m, 1H), 9.4 (s, 1H). 13C-NMR δ 25.93, 25.76, 27.89, 45.04, 160.90, 198.29.

1. temperatureThe reaction mixture was cooled with ice-water bath
2. extractionThe mixture was extracted with ethyl acetate (2×250 mL)
3. washThe extracts were washed with brine
4. dry with materialdried with sodium sulfate
5. customThe drying agent was removed by filtration
6. customthe solvent was removed

ORDレコード

ord-646dac1da50b4aa08f07a7fafed051fb

出典データセット

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06013830