HRID7592

反应详情

EQUATION

反应方程式

HRID 7592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (S)-{1-[3-(4-pyridin-2-ylpiperazin-1-yl)phenyl]ethyl}carbamic acid tert-butyl ester (4.1 g, 10.7 mmol) and hydrochloric acid (4N, 11 mL) in dioxane (40 mL) was stirred at 40° C. for 5 h. The reaction mixture was concentrated under vacuum, dissolved into water (50 mL), and washed with dichloromethane (2×50 mL). The aqueous layer was based with 5N NaOH and extracted with dichloromethane (3×100 mL). The combined organic layers were washed with brine (2×100 ml), dried over sodium sulfate and concentrated under vacuum to afford the title compound as an oil (2.70 g, 89% yield).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. dissolutiondissolved into water (50 mL)
  3. washwashed with dichloromethane (2×50 mL)
  4. extractionextracted with dichloromethane (3×100 mL)
  5. washThe combined organic layers were washed with brine (2×100 ml)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under vacuum