HRID1777354

反应详情

EQUATION

反应方程式

HRID 1777354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Carbon tetrabromide (1.6 gm, 0.0048 mol) is added to a stirred solution of 4-(3-hydroxypropyl) piperidine-1,4-dicarboxylic acid-1-tert-butyl ester-4-ethyl ester (1.27 gm, 0.0040 mol) and triphenyl phosphine (1.6 gm, 0.0060 mol) in dichloromethane (15 mL) at 0-5° C. temperature. Reaction mixture is allowed to stir at room temperature for 30 minutes. Removal of solvent gives a crude residue which is purified by column chromatography (silica gel 230-400 mesh, ethyl acetate:n-hexane 3:7) to get 4-(3-bromopropyl)piperidine-1,4-dicarboxylic acid-1-tert-butyl ester-4-ethyl ester.

WORKUP

后处理

  1. customReaction mixture
  2. customRemoval of solvent
  3. customgives a crude residue which
  4. customis purified by column chromatography (silica gel 230-400 mesh, ethyl acetate:n-hexane 3:7)