HRID1590886

反应详情

EQUATION

反应方程式

HRID 1590886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 g (1.2 mmol) of t-butyl [2-(2-bromo-5-phenyl-4-thiazolecarboxamido)ethyl]carbamate, 2 ml of trifluoroacetic acid and 10 ml of methylene chloride were heated to reflux for 2 hours and then evaporated. The residue was dissolved in methanol and treated with 1 ml of hydrobromic acid in glacial acetic acid (~30%). Renewed evaporation and recrystallization of the residue from methanol/ether yields 0.45 g (94.2%) of N-(2-aminoethyl)-2-bromo-5-phenyl-4-thiazolecarboxamide hydrobromide as biege crystals, melting point 214°-215° (dec.).

WORKUP

后处理

  1. temperatureto reflux for 2 hours
  2. customevaporated
  3. dissolutionThe residue was dissolved in methanol
  4. additiontreated with 1 ml of hydrobromic acid in glacial acetic acid (~30%)
  5. customRenewed evaporation and recrystallization of the residue from methanol/ether