HRID1768955

反应详情

EQUATION

反应方程式

HRID 1768955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(tert-butoxycarbonyl)piperazine (18.6 g, 100 mmol) and epichlorohydrine (10.2 ml, 12.0 g, 130 mmol) in methanol (50 ml) was stirred at room temperature for 24 hours and the solvent was evaporated. The residue was dissolved in 200 ml of ether and the solution was stirred with 10N aqueous NaOH (100 ml) at room temperature for 2 hours. Then the organic layer was separated, washed with brine until neutral, dried over MgSO4 and concentrated to afford the title compound (21.8 g) as a pale yellowish viscous oil, yield: 90.1%.

WORKUP

后处理

  1. customthe solvent was evaporated
  2. dissolutionThe residue was dissolved in 200 ml of ether
  3. customThen the organic layer was separated
  4. washwashed with brine until neutral,
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated