HRID656067
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
To a stirred solution of 5-bromo-6-fluoro-2,3-dihydro-1H-indole-7-carboxylic acid (5.8 g, 0.022 mol) in THF (120 mL) was added MnO2 (11.6 g, 0.134 mol). The reaction mixture was stirred at reflux overnight and then filtered (hot) through celite, washing with hot THF (2×75 mL). The filtrate was concentrated, giving a brown solid, which was suspended in 1M HCl (150 mL). The mixture stirred at reflux overnight to remove traces of Mn and then cooled to room temperature. The solid was filtered off, dried, and recrystallised from IPA, giving 3.5 g (61%) of the title compound.
WORKUP
后处理
- temperatureat reflux overnight
- filtrationfiltered (hot) through celite
- washwashing with hot THF (2×75 mL)
- concentrationThe filtrate was concentrated
- customgiving a brown solid, which
- stirringThe mixture stirred
- temperatureat reflux overnight
- customto remove traces of Mn
- filtrationThe solid was filtered off
- customdried
- customrecrystallised from IPA