HRID30173

反应详情

EQUATION

反应方程式

HRID 30173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Carboxymethyl-piperidine-1-carboxylic acid tert butyl ester (2.86 g) and sodium carbonate (0.62 g) were dissolved in water (30 ml) using gentle warming. A solution of 2-bromoacetophenone (2.33 g) in ethanol (60 ml) was then added and the mixture boiled for 2 h. the mixture was cooled to room temperature and stood for 16 h. The mixture was again boiled for 2 h. solvent removed at reduced pressure and the residue partitioned between water and ethyl acetate. The organic phase was dried (MgSO4) and solvent removed at reduced pressure. The residue was column chromatographed (silica gel, 1:1 ethyl acetate:pentane) to give the title compound (3.14 g).

WORKUP

后处理

  1. waitstood for 16 h
  2. waitThe mixture was again boiled for 2 h.
  3. customsolvent removed at reduced pressure
  4. customthe residue partitioned between water and ethyl acetate
  5. dry with materialThe organic phase was dried (MgSO4) and solvent
  6. customremoved at reduced pressure
  7. customchromatographed (silica gel, 1:1 ethyl acetate:pentane)