HRID1080698

反应详情

EQUATION

反应方程式

HRID 1080698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Methyl-2-(trimethylsilyl)-1H-indole-5-acetamide (8) (2.5 g, 0.00961 mol) was dissolved in CH3CN (50 mL) and HF (1.9 g of a 50% aqueous solution, 0.048 mol) was added. The mixture was stirred at RT for 1.5 h. The solvent was removed in vacuo and the residue was dissolved in EtOAc. The organic phase was extracted with saturated aqueous NaHCO3 and then with brine, dried over MgSO4, filtered and evaporated in vacuo. Silica gel chromatography (10-100% EtOAc gradient in hexane) of the concentrate afforded the product (0.86 g, 47.6%).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in EtOAc
  3. extractionThe organic phase was extracted with saturated aqueous NaHCO3
  4. dry with materialwith brine, dried over MgSO4
  5. filtrationfiltered
  6. customevaporated in vacuo