HRID74298

反应详情

EQUATION

反应方程式

HRID 74298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 2-(2-(4-methoxycarbonylphenylmethyl)aminonitrobenzen-5-yl)benzoxazole (see Working Example 113-2) (367 mg, 0.910 mmol) was added iron powder (102 mg, 1.82 mmol), 10% aqueous acetic acid (5 mL) and methanol (7 mL), and this was heated to reflux for 16 hours. After the reaction solution was cooled, saturated aqueous sodium hydrogen carbonate solution and chloroform were added, this was filtered through Celite, and the filtrate obtained was extracted. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The residue obtained was purified by silica gel column chromatography to yield the title compound (61.8 mg, 18% yield).

WORKUP

后处理

  1. temperaturethis was heated
  2. temperatureto reflux for 16 hours
  3. temperatureAfter the reaction solution was cooled
  4. filtrationthis was filtered through Celite
  5. customthe filtrate obtained
  6. extractionwas extracted
  7. customAfter the organic layer obtained
  8. dry with materialwas dried over anhydrous sodium sulfate, it
  9. filtrationwas filtered
  10. concentrationconcentrated
  11. customThe residue obtained
  12. customwas purified by silica gel column chromatography