反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Methyl 5-methyl-2-furoate (3.68 g, 26.29 mmol) in methanol (30 ml) was treated with a solution of potassium hydroxide (2.80 g, 50.0 mmol) in water (15 ml) and the mixture stirred for 2 h at room temperature. The methanol was evaporated in vacuo, the residue dissolved in water and washed with ethyl acetate. The aqueous phase was acidified with SN hydrochloric acid, and the product extracted with ethyl acetate (x3). The combined organic solutions were dried and concentrated to yield the title compound as a yellow solid (3.12 g, 94%); m.p. 110-112° C.; (Found: M+, 126.0312. C6H6O3 requires M+ 126.0317); νmax (CH2C12) 3300-2700, 1688, 1524, 1424, 1305, 1210 and 1167 cm-1 ; δH (CDCl3, 90 MHz) 2.40 (3 H, s), 6.15 (1 H, d, J 4 Hz) and 7.22 (1 H, d, J 4 Hz).
WORKUP
后处理
- customThe methanol was evaporated in vacuo
- dissolutionthe residue dissolved in water
- washwashed with ethyl acetate
- extractionthe product extracted with ethyl acetate (x3)
- customThe combined organic solutions were dried
- concentrationconcentrated