HRID349257

反应详情

EQUATION

反应方程式

HRID 349257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Heat a mixture of tri-n-butyl-phenylethynyl-stannane (11.0 g, 30.0 mmol) and 3,5-bis-trifluoromethyl-benzyl azide (9.68 g, 36.0 mmol) in toluene (40 mL) at reflux until reaction is complete. Concentrate to remove the solvent in vacuo and purify the residue by flash chromatography on silica gel (elution with 17% ether in hexanes) to give the title compound (17.5 g, 26.4 mmol, 88%). MS (ES) 660.1, 662.1 (M+1); LC Rf=0.1 (17% ether in hexanes).

WORKUP

后处理

  1. temperatureHeat
  2. temperatureat reflux until reaction
  3. concentrationConcentrate
  4. customto remove the solvent in vacuo
  5. custompurify the residue by flash chromatography on silica gel (elution with 17% ether in hexanes)