HRID1792077

反应详情

EQUATION

反应方程式

HRID 1792077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[1-[2-(1,3-Dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-7-yl)-phenyl]-1-methylsulfanylthiocarbonyloxymethyl]piperazine-1,4-dicarboxylic acid di-tert-butyl ester (low polarity) (0.175 g), tributyltin hydride (0.25 g), and 2,2′-azobis(isobutyronitrile) (0.010 g) were dissolved in toluene (5 ml) under nitrogen atmosphere, and the mixture was heated to reflux for 2 hours. The reaction mixture was cooled and the solvent was removed by distillation at reduced pressure. The residue was purified by silica gel column chromatography to give 0.123 g of the title compound from the elution fraction of hexane-ethyl acetate (1:1).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 2 hours
  3. temperatureThe reaction mixture was cooled
  4. customthe solvent was removed by distillation at reduced pressure
  5. customThe residue was purified by silica gel column chromatography