HRID1887707

反应详情

EQUATION

反应方程式

HRID 1887707 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 7.4 mL dioxane, 5.5 mL ethanol and 3.7 mL distilled water was added tert-butyl 4-(5-nitro-1H-indol-3-yl)-5,6-dihydropyridine-1(2H)-carboxylate (184 mg, 0.54 mmol). To the mixture was added powdered iron (0) (0.15 g, 5.0 eq) and ammonium chloride (0.885 g, 4.0 eq). The reaction was heated to 70° C. under argon for 3 h. The reaction was cooled and filtered and washed with MeOH. The solvent was removed to obtain the crude which was purified by silica gel chromatography to afford the desired compound tert-butyl 4-(5-amino-1H-indol-3-yl)-5,6-dihydropyridine-1(2H)-carboxylate.

WORKUP

后处理

  1. distillationTo a solution of 7.4 mL dioxane, 5.5 mL ethanol and 3.7 mL distilled water
  2. additionTo the mixture was added
  3. temperatureThe reaction was cooled
  4. filtrationfiltered
  5. washwashed with MeOH
  6. customThe solvent was removed
  7. customto obtain the crude which
  8. customwas purified by silica gel chromatography