HRID1418541
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
4-Bromo-6-fluoro-3-hydroxy-2-nitrobenzoic acid (22 mg 0.78 mmol) was dissolved in EtOH (10 mL) and PtS2 (2 mg) was added. Hydrogenation at room temperature and at atmospheric pressure for 14 h followed by filtration and evaporation gave a crude product. Purification by flash chromatography (SiO2, toluene-EtOAc-HOAc) afforded the product (4 mg). 1H NMR (CD3OD): δ 6.44 (d, J=11.3 Hz, 1 H); MS (EI, 70 eV): m/z (rel. int.) 249/251 (M+, 93/90).
WORKUP
后处理
- filtrationHydrogenation at room temperature and at atmospheric pressure for 14 h followed by filtration and evaporation
- customgave a crude product
- customPurification by flash chromatography (SiO2, toluene-EtOAc-HOAc)