HRID1792077
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureto reflux for 2 hours
- temperatureThe reaction mixture was cooled
- customthe solvent was removed by distillation at reduced pressure
- customThe residue was purified by silica gel column chromatography