HRID417985

反应详情

EQUATION

反应方程式

HRID 417985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1-Methylhomopiperazine (2.00 g, 17.5 mmol) and DIPEA (3.0 mL, 18.4 mmol) were dissolved in DMF (25 mL). 2-bromethanol (1.3 mL, 18.4 mmol) was added slowly over 5 minutes. The reaction mixture was stirred at 100° C. for 2 hours and then at room temperature for 48 hours and then concentrated in vacuo. The residue was dissolved in EtOAc (−300 mL) and then washed sequentially with 1M aq Na2CO3 solution (5×200 mL), dried (MgSO4) and concentrated in vacuo to give 2-(4-methylhomopiperazin-1-yl)ethanol (2.77 g, 100%) as a brown oil which was used without further purification.

WORKUP

后处理

  1. waitat room temperature for 48 hours
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in EtOAc (−300 mL)
  4. washwashed sequentially with 1M aq Na2CO3 solution (5×200 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo