HRID733517
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
To a solution of methyl 8-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylate (10 g, 0.048 mol) in MeOH (100 ml) was added hydroxylamine hydrochloride (5 g, 0.07 mol), followed by sodium acetate (6 g, 0.072 mol). The reaction mixture was stirred at rt for 1 h and heated to 50° C. for 15 h. The solvent was removed under vacuum and the residue was diluted with water. The product was extracted with EtOAc (2×150 ml), dried and evaporated to yield 10 g (93%) of the titled compound as a solid. TLC-Chloroform/MeOH (9/1), Rf=0.3.
WORKUP
后处理
- temperatureheated to 50° C. for 15 h
- customThe solvent was removed under vacuum
- additionthe residue was diluted with water
- extractionThe product was extracted with EtOAc (2×150 ml)
- customdried
- customevaporated