HRID1792011

反应详情

EQUATION

反应方程式

HRID 1792011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-[3-Methyl-7-(2-butynyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester (0.30 g) and potassium carbonate (0.21 g) were dissolved in N,N-dimethylformamide (10 ml), and 2-(2-bromoethoxy)tetrahydro-2H-pyran (0.23 ml) was added thereto. After stirring at room temperature overnight, the reaction mixture was diluted with ethyl acetate, washed with water, and dried over magnesium sulfate. After removing the solvent by distillation, ethanol (10 ml) and pyridinium p-toluenesulfonate (60 mg) were added to the resulting residue, and the reaction mixture was stirred at 60° C. for 3 hours. The reaction solution was distilled. The residue was purified by silica gel column chromatography to obtain 0.14 g of the title compound from a fraction eluted with hexane-ethyl acetate (1:5).

WORKUP

后处理

  1. washwashed with water
  2. dry with materialdried over magnesium sulfate
  3. customAfter removing the solvent
  4. distillationby distillation, ethanol (10 ml) and pyridinium p-toluenesulfonate (60 mg)
  5. additionwere added to the resulting residue
  6. stirringthe reaction mixture was stirred at 60° C. for 3 hours
  7. distillationThe reaction solution was distilled
  8. customThe residue was purified by silica gel column chromatography