反应详情

To methyl 3,4,6-Trichloropicolinate (3.57 g, 14.85 mmol) in 20 mL of methanol was added 1N NaOH (14.85 mL, 14.85 mmol). The reaction mixture was stirred at room temperature for 1 hr and then concentrated to dryness in vacuo. 100 mL each of diethyl ether and H2O were added. Aqueous layer was acidified with 1N HCl until pH=2. Methylene chloride was added and the aqueous phase was extracted with additional CH2Cl2 (2×100 mL). The combined extracts were dried (MgSO4) and concentrated to give 3.13 g of a white solid. 1H NMR(CDCl3): δ 7.50 (s, 1H).

1. concentrationconcentrated to dryness in vacuo
2. addition100 mL each of diethyl ether and H2O were added
3. additionMethylene chloride was added
4. extractionthe aqueous phase was extracted with additional CH2Cl2 (2×100 mL)
5. dry with materialThe combined extracts were dried (MgSO4)
6. concentrationconcentrated