HRID895715

反应详情

EQUATION

反应方程式

HRID 895715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (t-butyl 2-(6-cyano-2-naphthyloxy)-5-nitrobenzoate) (760 mg) obtained in a previous production example, iron powder (718 mg) and ammonium chloride (73 mg) were heated to reflux in ethanol:water (3:1, 30 ml) and reacted for 30 minutes. The insoluble portion was immediately filtered using celite, and the filtrate was concentrated. A saturated sodium bicarbonate solution was added to the obtained residue, and extraction was performed with ethyl acetate. The ethyl acetate layer was washed with saturated saline and then dried over magnesium sulfate, and the solvent was distilled off to obtain 736 mg of t-butyl 5-amino-2-(6-cyano-2-naphthyloxy)benzoate.

WORKUP

后处理

  1. temperaturewere heated
  2. customreacted for 30 minutes
  3. filtrationThe insoluble portion was immediately filtered
  4. concentrationthe filtrate was concentrated
  5. additionA saturated sodium bicarbonate solution was added to the obtained residue, and extraction
  6. washThe ethyl acetate layer was washed with saturated saline
  7. dry with materialdried over magnesium sulfate
  8. distillationthe solvent was distilled off