HRID1270754

反应详情

EQUATION

反应方程式

HRID 1270754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A suspension of 7-nitro-2-aminonaphthalene (260 mg, 1.38 mmol) in concentrated HCl (10 mL) is cooled to 0° C. Sodium nitrite (105 mg, 1.53 mmol) is added in portions and the reaction is allowed to stir at 0° C. for 30 minutes. A solution of iodide (175 mg, 253.8 mmol) and potassium iodide (459 mg, 2.76 mmol) in water (5 mL) is added dropwise. After stirring at 0° C. for 1 hour, the solid is removed by filtration. The solid is dissolved in EtOAc and washed with sodium metabisulfite solution, water and brine. The organic layer is dried (Na2SO4) and the solvents evaporated to give 2-iodo-7-nitronaphthalene as an orange solid.

WORKUP

后处理

  1. stirringAfter stirring at 0° C. for 1 hour
  2. customthe solid is removed by filtration
  3. dissolutionThe solid is dissolved in EtOAc
  4. washwashed with sodium metabisulfite solution, water and brine
  5. dry with materialThe organic layer is dried (Na2SO4)
  6. customthe solvents evaporated