HRID34936

反应详情

EQUATION

反应方程式

HRID 34936 的结构方程式

PROCEDURE

实验过程

3.2 g of t-butyl [2-(3-bromopyridine-2-carboxamido)ethyl]carbamate were heated to reflux for 4 hours with 3.5 ml of methylene chloride and 3.5 ml of trifluoroacetic acid. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in ethanol and the solution was treated with an equimolar amount of ethanolic hydrochloric acid. The hydrochloride was recrystallized from methanol/ether, whereby there was obtained N-(2-aminoethyl)-3-bromopyridine-2-carboxamide hydrochloride as white crystals, m.p. 279°.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in ethanol
  3. additionthe solution was treated with an equimolar amount of ethanolic hydrochloric acid
  4. customThe hydrochloride was recrystallized from methanol/ether