HRID895715
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 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
- temperaturewere heated
- customreacted for 30 minutes
- filtrationThe insoluble portion was immediately filtered
- concentrationthe filtrate was concentrated
- additionA saturated sodium bicarbonate solution was added to the obtained residue, and extraction
- washThe ethyl acetate layer was washed with saturated saline
- dry with materialdried over magnesium sulfate
- distillationthe solvent was distilled off