HRID16752

反应详情

EQUATION

反应方程式

HRID 16752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 4-(2-[dimethylamino]ethylamino)benzoate (1.00 g, 4.50 mmol) was dissolved in THF (30 ml). (2-Methylpropan-2-yl)oxycarbonyl tert-butyl carbonate (1.035 g, 4.72 mmol) was added and the solution was refluxed for 3 h. The solvent was then evaporated, the residue was dissolved in DCM, washed with sat. aq. ammonium chloride solution, dried over sodium sulphate, filtered and evaporated to give methyl 4-[2-dimethylaminoethyl-[tert-butoxycarbonyl]amino]benzoate (1.07 g, 74%) as a brown oil.

WORKUP

后处理

  1. temperaturethe solution was refluxed for 3 h
  2. customThe solvent was then evaporated
  3. dissolutionthe residue was dissolved in DCM
  4. washwashed with sat. aq. ammonium chloride solution
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated