HRID2262477

反应详情

EQUATION

反应方程式

HRID 2262477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-methoxycarbonylmethylpiperazine-1,4-dicarboxylic acid di-tert-butyl ester (662 mg, 1.85 mmol) in anhydrous THF (10 mL) at 0° C. was slowly added a 1M solution of LiAlH4 in THF (5.7 mL, 5.70 mmol). The stirred reaction mixture was allowed to warm to room temperature over a period of 15 minutes before being refluxed for 2 hours. After this time the reaction mixture was cooled to 0° C. and cautiously quenched by the dropwise addition of 1.0M aqueous NaOH solution until the effervescing ceased. The resulting gel was diluted with THF (50 mL) and the solids filtered off. The filtrate was concentrated in vacuo to afford 2-(1,4-dimethylpiperazin-2-yl)ethanol (191 mg, 65%) as a colourless oil.

WORKUP

后处理

  1. customThe stirred reaction mixture
  2. temperaturebefore being refluxed for 2 hours
  3. temperatureAfter this time the reaction mixture was cooled to 0° C.
  4. customcautiously quenched by the dropwise addition of 1.0M aqueous NaOH solution until the effervescing
  5. additionThe resulting gel was diluted with THF (50 mL)
  6. filtrationthe solids filtered off
  7. concentrationThe filtrate was concentrated in vacuo