HRID1106861

反应详情

EQUATION

反应方程式

HRID 1106861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2-(4-nitrophenoxy)ethyl bromide (0.5 g, 2.03 mmol) was dissolved in methanol (30 ml) and, after adding 10% Pd/C (0.2 g), the solution was stirred for 1 h in hydrogen gas, followed by filtration. The filtrate was concentrated under vacuum and the residue was dissolved in pyridine (20 ml). To the resulting solution, methanesulfonyl chloride (0.25 ml, 3.2 mmol) was slowly added dropwise, followed by stirring overnight. Water was poured into the reaction mixture, followed by extraction with ethyl acetate and concentration under vacuum. The residue was subjected to column chromatography using a 1:1 solvent system of ethyl acetate and hexane as an eluent to yield the end compound 2-(4-methanesulfonamidophenoxy)ethyl bromide (0.22 g).

WORKUP

后处理

  1. filtrationfollowed by filtration
  2. concentrationThe filtrate was concentrated under vacuum
  3. dissolutionthe residue was dissolved in pyridine (20 ml)
  4. extractionfollowed by extraction with ethyl acetate and concentration under vacuum