HRID1418541

反应详情

EQUATION

反应方程式

HRID 1418541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationHydrogenation at room temperature and at atmospheric pressure for 14 h followed by filtration and evaporation
  2. customgave a crude product
  3. customPurification by flash chromatography (SiO2, toluene-EtOAc-HOAc)