HRID18214

反应详情

EQUATION

反应方程式

HRID 18214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the 2-amino-3-(bromomethyl)-5-bromopyridine hydrobromide salt (prepared above) in 40% aqueous methylamine (50 mL) and THF (50 mL) was stirred at RT overnight in a pressure bottle. The reaction solution was concentrated and extracted with EtOAc (2×100 mL). The combined organic phases were washed with H2O, dried over Na2SO4 and concentrated. Purification on silica gel afforded the title compound (4.25 g, 80%) as a yellow oil: MS (ES) m/e 217 (M+H)+.

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated
  2. extractionextracted with EtOAc (2×100 mL)
  3. washThe combined organic phases were washed with H2O
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customPurification on silica gel