Hydrochloric Acid → (1R,2R)-2-(3,4-Difluorophenyl)cyclopropanecarboxylic acid

関与物質

反応条件

反応手順

(1R,2R)-2-(3,4-difluorophenyl)cyclopropanecarbonitrile (5 g), ethanol (25 mL) were charged to a round bottom flask followed by addition of caustic lye (10 mL). The reaction mixture was heated to 80-85° C. and maintained at the same temperature for 2-3 hours till the completion of reaction as monitored by TLC. The reaction mixture was cooled to 25-30° C. and then water (15 mL) was added to the mixture. The pH of the mixture was adjusted to 1-2 with conc. hydrochloric acid (15 mL) followed by addition of ethyl acetate (25 mL). The layers were separated and aqueous layer was extracted with ethyl acetate (25 mL). The organic layers were combined and charged with water (15 mL) and caustic lye (10 mL). After stirring, the organic layer was separated and pH of the aqueous layer was adjusted to 1-2 with conc. hydrochloric acid (10 mL). To this ethyl acetate (25 mL) and water (15 mL) were added and stirred for 10-15 minutes. The layers were separated and the aqueous layer was extracted with ethyl acetate (25 mL). The organic layers were combined and washed with water (2×15 mL) followed by complete distillation of solvent from organic layer under vacuum at 50-55° C. to afford the title compound in about 94.3% yield having HPLC purity of about 99%.

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