HRID747723

反应详情

EQUATION

反应方程式

HRID 747723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

5.5 g (11.3 mmol) of benzyl 4-[4-[(2S)-2-(t-butoxycarbonylamino)-3-hydroxypropyl]phenoxy]piperidine-1-carboxylate was dissolved in 60 ml of dichloromethane. 3.2 ml (22.6 mmol) of triethylamine and 1.95 g (17.0 mmol) of methanesulfonyl chloride were added to the solution at 0° C. After stirring for 4 hours, the reaction mixture was treated with dichloromethane as the extractant in an ordinary manner to obtain an oily residue. The residue thus obtained was dissolved in 120 ml of dimethylformamide. 2.57 g (60.6 mmol) of lithium chloride was added to the solution, and they were stirred at 50° C. for 15 hours. After the treatment with ethyl acetate as the extractant in an ordinary manner, the crude product was obtained, which was purified by the silica gel column chromatography to obtain the title compound.

WORKUP

后处理

  1. customto obtain an oily residue
  2. customThe residue thus obtained
  3. stirringwere stirred at 50° C. for 15 hours
  4. customwhich was purified by the silica gel column chromatography