HRID2262467

反应详情

EQUATION

反应方程式

HRID 2262467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

(S)-2-hydroxymethyl-piperazine-1,4-dicarboxylic acid di-tert-butyl ester (5.66 g, 17.9 mmol) was dissolved in THF (10 mL) and cooled to 0° C. 2M LiAlH4 in THF (28.5 mL, 57.0 mmol) was added. The reaction mixture was stirred at reflux for 4 hours and then cooled to 0° C. and quenched with the drop-wise addition of 1M sodium hydroxide solution (20 mL). The reaction mixture was diluted with THF (50 mL), filtered and the filtrate was concentrated in vacuo to give 1,4-dimethyl-(S)-2-hydroxymethyl piperazine (1.44 g, 56%) as a colourless oil which was used without further purification.

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. temperaturecooled to 0° C.
  3. customquenched with the drop-wise addition of 1M sodium hydroxide solution (20 mL)
  4. additionThe reaction mixture was diluted with THF (50 mL)
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated in vacuo