反应详情

A mixture of methyl 3-methyl-5-pentanoylbenzoate (LXXVI, step 2. 133 mg, 0.605 mmol) in methanol (1 mL) is stirred with tetrahydrofuran/methanol/sodium hydroxide (2 N) (3/1/1, 3 mL) for 3 days. The reaction mixture is diluted with ethyl acetate and washed with water. The aqueous phase is separated and acidified with hydrochloric acid (1 N) and extracted with methylene chloride. The organic phase is dried (sodium sulfate), filtered, and concentrated under reduced pressure to give 3-methyl-5-pentanoylbenzoic acid (IX–LXXVII), NMR (300 MHz, CD3OD): δ 8.44, 8.03, 3.10, 2.33, 1.78, 1.64 and 1.34.

1. washwashed with water
2. customThe aqueous phase is separated
3. extractionextracted with methylene chloride
4. dry with materialThe organic phase is dried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure