HRID1924888

反应详情

EQUATION

反应方程式

HRID 1924888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

PROCEDURE

实验过程

A mixture of N-(2-diethylaminoethyl)-4-nitrobenzenesulfonamide (0.72 g, 2.13 mmol) in cyclohexene (4.8 mL) and EtOH (24 mL) is heated using an oil bath until dissolution had almost been achieved. At this point Pd on C (144 mg, 10% (w/w)) is added, and the mixture heated at reflux for 5 hours. After this time the solution is cooled to room temperature, then filtered through Hy-flo. The filtrate is evaporated in vacuo to afford a yellow gum. The yellow gum is dissolved in the minimum quantity of methanol, then NaHCO3 (1 eq.) dissolved in water, is added. The mixture is stirred at room temperature, then the mixture extracted with EtOAc (2×). The combined organic layers are dried (MgSO4), and evaporated to afford the title aniline.

WORKUP

后处理

  1. temperatureis heated
  2. dissolutionuntil dissolution
  3. temperaturethe mixture heated
  4. temperatureat reflux for 5 hours
  5. filtrationfiltered through Hy-flo
  6. customThe filtrate is evaporated in vacuo
  7. customto afford a yellow gum
  8. additionis added
  9. extractionthe mixture extracted with EtOAc (2×)
  10. dry with materialThe combined organic layers are dried (MgSO4)
  11. customevaporated