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Methyl 5-methoxyvalerate (7.33 g, 50.2 mmol) and KOH (14.4 g, 0.256 mol) were dissolved into a mixture of 50 ml of water and 150 ml of MeOH. The solution was stirred at 0° C. for 2 hrs then MeOH was removed in vacuo. After washed by CHCl3 (50 ml), the aqueous layer was acidified to pH=1 by 2N HCl and extracted by Et2O (2×100 ml). Organic layers were combined, washed with water (100 ml) and dried over Na2SO4. After filtration and evaporation of solvent, 5-methoxyvaleric acid (5.27 g, 79.6%) was obtained as a colorless oil.

1. customMeOH was removed in vacuo
2. washAfter washed by CHCl3 (50 ml)
3. extractionextracted by Et2O (2×100 ml)
4. washwashed with water (100 ml)
5. dry with materialdried over Na2SO4
6. filtrationAfter filtration and evaporation of solvent