HRID844204
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
A stirred solution of methyl 6-chloro-7-fluoroindole-2-carboxylate (2.3 g, 10 mmol), tetrahydrofuran (20 mL) and aqueous sodium hydroxide solution (2 N, 20 mL) was heated under reflux for 16 h. The mixture was cooled to room temperature and partitioned between aqueous sulfiuric acid (2 M, 30 mL) and ethyl acetate (3×30 mL). The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo to give the product (2.1 g, 98% yield) as a white solid: IR νmax (Nujol)/cm−1 1681, 1557, 1263, 1206, 926 and 840; NMR δH (400 MHz, DMSO-d6) 7.01-7.12 (2H, m) and 7.31-7.34 (1H, m).
WORKUP
后处理
- temperatureunder reflux for 16 h
- custompartitioned between aqueous sulfiuric acid (2 M, 30 mL) and ethyl acetate (3×30 mL)
- dry with materialThe combined organic extracts were dried (magnesium sulfate)
- concentrationconcentrated in vacuo