HRID566964
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
O-Benzyl hydroxylamine hydrochloride (0.8 g, 6.5 mmol) was added to a suspension of 3-nitro-1,8-naphthalic anhydride (1.0 g, 4.1 mmol) in pyridine (20 mL). The mixture was refluxed for 3 hours and concentrated in vacuo. The solid residue obtained was purified by column chromatography (silica gel using 2% methanol in chloroform). Fractions containing the target compound were combined, concentrated, and dried to give 1.3 g of the title compound. mp 239-241° C.;
WORKUP
后处理
- temperatureThe mixture was refluxed for 3 hours
- concentrationconcentrated in vacuo
- customThe solid residue obtained
- customwas purified by column chromatography (silica gel using 2% methanol in chloroform)
- additionFractions containing the target compound
- concentrationconcentrated
- customdried