HRID16825

反应详情

EQUATION

反应方程式

HRID 16825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of tert-butyl 4-cyclobutylpiperazine-1-carboxylate (1.1553 g, 4.81 mmol) in ethyl acetate (10 mL) and methanol (10.00 mL) was treated with a 4M-solution hydrogen chloride in dioxane (1.669 mL, 48.07 mmol) was stirred at room temperature for 40 h under nitrogen. The reaction was incomplete so f 4M-solution hydrogen chloride in dioxane (10 mL) was added and the solution was stirred at room temperature for a further 2 h. The reaction mixture was evaporated to dryness to afford a solid. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 3.5M NH3/MeOH and pure fractions were evaporated to dryness to afford 1-cyclobutylpiperazine (0.571 g, 85%) as a yellow oil.

WORKUP

后处理

  1. additionwas added
  2. stirringthe solution was stirred at room temperature for a further 2 h
  3. customThe reaction mixture was evaporated to dryness
  4. customto afford a solid
  5. customThe crude product was purified by ion exchange chromatography
  6. washThe desired product was eluted from the column
  7. customwere evaporated to dryness