HRID514784

反应详情

EQUATION

反应方程式

HRID 514784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Compound 65 (0.336 g, 1.00 mmol) was dissolved in PhNO2 (7 mL). The solution was cooled down in an ice bath. Then, AlCl3 (0.67 g, 5.02 mmol) and after that, AcCl (0.36 mL, 5.04 mmol) were added. The resulting mixture was kept for 40 min (LC/MS monitoring), diluted with water, neutralized with aqueous NaHCO3 solution, extracted with CHCl3, and evaporated. The product was purified on a short thick column, eluent: 100:0→90:10. Yield of product: 0.307 g (82%) (R); S-isomer was obtained similarly (77%).

WORKUP

后处理

  1. temperatureThe solution was cooled down in an ice bath
  2. extractionextracted with CHCl3
  3. customevaporated
  4. customThe product was purified on a short thick column, eluent
  5. customS-isomer was obtained similarly (77%)