Hydrochloric Acid → 3-Methylisoxazole-5-carboxylic acid

関与物質

反応手順

A round bottom flask with magnetic stirrer was charged with 3-methyl-isoxazole-5-carboxylic acid ethyl ester (900 mg, 5.8 mmol) in tetrahydrofuran (2.0 mL). To the reaction was added a solution of sodium hydroxide (465 mg, 11.6 mmol) in water (2 mL), followed by methanol (4 mL). The reaction was stirred at room temperature for 18-20 hours under an argon atmosphere. The reaction was transferred to a separatory funnel and the pH adjusted to 2 via addition of 1N hydrochloric acid. The mixture was extracted with ethyl acetate (3×35 mL) and the combined extractions were washed with brine (1×50 mL), dried over magnesium sulfate, and filtered. The filtrate was concentrated in vacuo to yield 3-methyl-isoxazole-5-carboxylic acid as a white solid (660 mg, 90%). The solid was used without purification in the next reaction.

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