HRID1494432
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
7-Fluoro-1-methylindole-3-carboxaldehyde (1.0 g) was dissolved in t-butanol (50 ml). 1.25M Sodium hydrogen phosphate (20 ml) was added followed by 1.0M potassium permanganate (30 ml), and the mixture was stirred at 20 for 16h. 2M Hydrochloric acid (200 ml) was then added and the mixture was extracted with ethyl acetate (2×200 ml). The combined, dried organic extracts were evaporated in vacuo to leave a solid which was purified by FCC eluting with hexane:ether (1:1) followed by hexane:ether:acetic acid (50:50:1) to give the title compound (192 mg), m.p. 225°-227°.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate (2×200 ml)
- customdried organic extracts were evaporated in vacuo
- customto leave a solid which
- customwas purified by FCC
- washeluting with hexane:ether (1:1)