HRID278953

反应详情

EQUATION

反应方程式

HRID 278953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was refluxed for 3 hours
  2. concentrationconcentrated in vacuo
  3. customThe solid residue obtained
  4. customwas purified by column chromatography (silica gel using 2% methanol in chloroform)
  5. additionFractions containing the target compound
  6. concentrationconcentrated
  7. customdried