HRID2056775

反应详情

EQUATION

反应方程式

HRID 2056775 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 2-((1S)-6-bromo-3,4-dihydro-1H-2-benzopyran-1-yl)ethanol (0.815 g, 3.17 mmol) in dry dioxan (5 mL) was added 1,3-oxazolidin-2-one (0.26 g, 2.95 mmol), trans-1,2-cyclohexanediamine (0.05 mL, 0.42 mmol), copper(I) iodide (0.040 g, 0.21 mmol) and potassium carbonate (1.02 g, 7.36 mmol), and the mixture heated at reflux under nitrogen overnight. 2M Ammonia was added and the mixture extracted into dichloromethane. The combined organic extracts were dried (MgSO4), filtered and evaporated in vacuo. The crude product was purified by flash chromatography on silica to yield the title compound.

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux under nitrogen overnight
  3. extractionthe mixture extracted into dichloromethane
  4. dry with materialThe combined organic extracts were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe crude product was purified by flash chromatography on silica