HRID1091659
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe solvent was evaporated
- dissolutionThe residue was dissolved in water (200 mL)
- extractionThe solution was extracted with EA (3×100 mL)
- washthe combined EA extracts were washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated