HRID1819689
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
Step J (2): To a solution of methyl 2-(5-bromo-2-cyano-1H-indol-3-yl)acetate (50 mg, 0.17 mmol) in THF (1.0 mL) was added a solution of LiOH (12 mg, 0.5 mmol) in water (0.5 mL). The mixture was stirred at rt for 3 h. 100 mL of EtOAc was added, and the resulting solution was washed with 0.1 N HCl and water. The organic layer was dried over Na2SO4, and the solvents was removed to give 45 mg of the title compound 2-(5-bromo-2-cyano-1H-indol-3-yl)acetic acid (yield 94.7%) which was used without further purification. 1H NMR (500 MHz, CDCl3) δ ppm 3.89 (s, 2 H) 7.34 (d, J=8.85 Hz, 1 H) 7.43 (dd, J=8.85, 1.83 Hz, 1 H) 7.83 (d, J=1.53 Hz, 1 H).
WORKUP
后处理
- washthe resulting solution was washed with 0.1 N HCl and water
- dry with materialThe organic layer was dried over Na2SO4
- customthe solvents was removed