HRID1091659

反应详情

EQUATION

反应方程式

HRID 1091659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The tert-butyl 4-amino-3-nitrophenyl(ethyl)carbamate from the previous step was dissolved in dioxane (35 mL) and hydrogen chloride (35 mL of a 4M solution in dioxane) was added. The mixture was stirred at room temperature for 18 hr and then the solvent was evaporated. The residue was dissolved in water (200 mL) and the solution adjusted to pH10 with 5M sodium hydroxide solution. The solution was extracted with EA (3×100 mL), and the combined EA extracts were washed with brine, dried over magnesium sulfate, and concentrated to give N1-ethyl-3-nitrobenzene-1,4-diamine as a purple solid (1.68 g).

WORKUP

后处理

  1. customthe solvent was evaporated
  2. dissolutionThe residue was dissolved in water (200 mL)
  3. extractionThe solution was extracted with EA (3×100 mL)
  4. washthe combined EA extracts were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated