HRID240771

反应详情

EQUATION

反应方程式

HRID 240771 的结构方程式

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

2-Ethynyl toluene (456 μL, 3.62 mmol) was added to 1,1,1-tributyl-N,N-dimethylstannanamine (1.21 g, 3.62 mmol), and the mixture was stirred in a sealed vial at 70° C. for 3 hours. The mixture was cooled to ambient temperature, and the vial was stirred unsealed for 10 minutes. Benzyl azide (678 μL, 5.42 mmol) was added, and the vial was resealed and heated to 130° C. overnight. The mixture was purified by silica gel chromatography eluting with a gradient of 5-45% ethyl acetate in hexanes to afford the title compound. MS (ESI+) m/z 539.8 (M+H)+.

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. stirringthe vial was stirred unsealed for 10 minutes
  3. temperatureheated to 130° C. overnight
  4. customThe mixture was purified by silica gel chromatography
  5. washeluting with a gradient of 5-45% ethyl acetate in hexanes