HRID1184990

反应详情

EQUATION

反应方程式

HRID 1184990 的结构方程式

PROCEDURE

实验过程

4-Hydroxy-2,2,6,6-tetramethylpiperidine-N-oxyl (1.9 g, 11 mmol) is dissolved in THF (40 ml) and hydrogenated in the presence of 0.035 g Pt (5% on carbon) catalyst using 4 bar hydrogen pressure. The hydrogen uptake stops after approximately one hour. The reaction mixture is then filtered and mixed with the solution of bis-p-tolyl-carbodiimide (2.45 g, 11 mmol) in THF (30 ml). The solution is stirred under argon at room temperature for 16 hours and concentrated. The residue is chromatographed on silica gel with hexane-ethyl acetate (1:1) and the pure fractions are crystallized from ethyl acetate to afford 1.6 g of the title compound as a colorless solid, mp. 124-126° C.

WORKUP

后处理

  1. filtrationThe reaction mixture is then filtered
  2. concentrationconcentrated
  3. customThe residue is chromatographed on silica gel with hexane-ethyl acetate (1:1)
  4. customthe pure fractions are crystallized from ethyl acetate