HRID1504945
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 solution of compound 24 (800 mg, 3.25 mmol) in EtOH (10 mL) was added concentrated HCl solution (12N, 5 mL). The mixture was heated at reflux for 1 h, cooled to room temperature, concentrated in vacuo. The resulting white solid was dissolved in EtOAc, washed with saturated aqueous NaHCO3, dried over Na2SO4 and concentrated to give compound 25 (660 mg, 99%) as a light yellow solid. 1H NMR (400 MHz, CDCl3) δ7.40 (d, 1H, J=7.2 Hz), 7.09 (d, 1H, J=10.0 Hz), 4.48 (br s, 2H).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux for 1 h
- concentrationconcentrated in vacuo
- dissolutionThe resulting white solid was dissolved in EtOAc
- washwashed with saturated aqueous NaHCO3
- dry with materialdried over Na2SO4
- concentrationconcentrated