HRID866251

反应详情

EQUATION

反应方程式

HRID 866251 的结构方程式

PROCEDURE

实验过程

3-Nitro-1,2-phenylenediamine (0.065 moles, 10.2 g) was added to 200 ml formic acid and heated to reflux for 3 hours. The solution was cooled and then concentrated under vacuum. The residue was dissolved in water. The pH was adjusted to 8.3 using 5N sodium hydroxide. The intermediate was extracted with ethyl acetate. The organic phase was washed with brine, dried over sodium sulfate and concentrated to yield 7.0 g of 4-nitrobenzimidazole. (MS)

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 3 hours
  3. temperatureThe solution was cooled
  4. concentrationconcentrated under vacuum
  5. dissolutionThe residue was dissolved in water
  6. extractionThe intermediate was extracted with ethyl acetate
  7. washThe organic phase was washed with brine
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated