HRID1594930

反应详情

EQUATION

反应方程式

HRID 1594930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-[5-(2-amino-ethyl)-imidazol-1-ylmethyl]-2-fluoro-benzonitrile dihydrochloride (0.92 g, 0.0029 mmol) in acetonitrile (150 mL) and triethylamine (3.2 mL) was added 2-bromoethyl ether (0.839 mL, 0.0067 mmol) and the mixture was refluxed for 48 hr. The solvents were removed in vacuo and the residue was dissolved in EtOAc which was washed twice with 1M HCl (100 mL). The HCl layers were combined and adjusted to pH=9 with solid Na2CO3 and extraxcted 3 times with EtOAc. The EtOAc layers were combined and dried with brine and MgSO4. Removal of the EtOAc in vacuo yielded the title compound.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 48 hr
  2. customThe solvents were removed in vacuo
  3. dissolutionthe residue was dissolved in EtOAc which
  4. washwas washed twice with 1M HCl (100 mL)
  5. dry with materialdried with brine and MgSO4
  6. customRemoval of the EtOAc in vacuo