HRID6946

反应详情

EQUATION

反应方程式

HRID 6946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

282 mg of indole (2.4 mmol) were dissolved in 10 ml of CH3OH and 5 ml of H2O; 102 mg of semisuccinic aldehyde (1 mmol) and 240 mg of dysprosium triflate-(CF3SO3)3Dy-(0.393 mmol) were added. The resulting solution was stirred at 35° C. for 24 hours. At the end of that period the methanol was removed under vacuum and the residue was extracted with ethyl acetate (3×50 ml). The organic extracts were pooled, washed with a small amount of water, dried on anhydrous Na2SO4, filtered and concentrated to dryness. The end product was isolated and purified chromatographically on an SiO2 column, using a hexane:isopropyl alcohol gradient ranging from 9:1 to 8:2.

WORKUP

后处理

  1. customAt the end of that period the methanol was removed under vacuum
  2. extractionthe residue was extracted with ethyl acetate (3×50 ml)
  3. washwashed with a small amount of water
  4. dry with materialdried on anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated to dryness
  7. customThe end product was isolated
  8. custompurified chromatographically on an SiO2 column