HRID2210942

反应详情

EQUATION

反应方程式

HRID 2210942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 19.8 g (95 mmol) of 2-(N-(t-butyloxycarbonyl)aminomethyl)pyridine in anhydrous tetrahydrofuran was cooled under N2 atmosphere to 0° C. and treated with 4.95 g (124 mmol) of sodium hydride (60% dispersion in oil). The solution was stirred for 15 min, treated dropwise with 7.1 ml (114 mmol) of methyl iodide, stirred at ambient temperature for 2 h, and quenched cautiously with water. The resulting mixture was partitioned between ether and water, dried over Na2SO4, and concentrated in vacuo. Chromatography on silica gel provided 14.9 g (70%) of the desired compound as a colorless oil.

WORKUP

后处理

  1. stirringstirred at ambient temperature for 2 h
  2. customquenched cautiously with water
  3. customThe resulting mixture was partitioned between ether and water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo