HRID1036407

反应详情

EQUATION

反应方程式

HRID 1036407 的结构方程式

PROCEDURE

实验过程

(R)-4-(6-Hydroxynaphthalen-2-yl)-4-methyl-oxazolidin-2-one (0.1042 g, 0.0004284 mol) was dissolved in tetrahydrofuran (5.00 mL, 0.0616 mol) in a capped 40 mL vial. 4-Trifluoromethylcyclohexanol (0.101 g, 0.000600 mol) was added, followed by triphenylphosphine (0.180 g, 0.000685 mol) and the mixture was refluxed for 5 minutes. Diisopropyl azodicarboxylate (0.135 mL, 0.000685 mol) was then added and the mixture was heated at reflux overnight. TLC analysis showed that the reaction was complete. The mixture was concentrated to dryness under vacuum and purified by flash chromatography (0-20% EtOAc in methylene chloride).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 5 minutes
  2. temperaturethe mixture was heated
  3. temperatureat reflux overnight
  4. concentrationThe mixture was concentrated to dryness under vacuum
  5. custompurified by flash chromatography (0-20% EtOAc in methylene chloride)