HRID441021

反应详情

EQUATION

反应方程式

HRID 441021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chlorobenzoxazole (23.04 g) was added dropwise to an ice-cooled solution of 2-(isopropylamino)ethanol (15.45 g) and triethylamine (30.3 g) in tetrahydrofuran (500 ml). The mixture was stirred at room temperature for 30 minutes, then heated at reflux overnight before being cooled and evaporated. The residue was dissolved in dichloromethane (800 ml) and washed with saturated sodium bicarbonate solution (500 ml), water (3×11) brine (11), dried (MgSO4), filtered and evaporated. The title compound was obtained as an oil following chromatography on silica gel using 1.5% methanol-dichloromethane as solvent.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux overnight
  3. temperaturebefore being cooled
  4. customevaporated
  5. dissolutionThe residue was dissolved in dichloromethane (800 ml)
  6. washwashed with saturated sodium bicarbonate solution (500 ml), water (3×11) brine (11)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customevaporated