HRID638130

反应详情

EQUATION

反应方程式

HRID 638130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Alcohol 5 (7.7 g, 68.75 mmol) was dissolved in 75 mL dry ether and cooled to 0°. A few crystals of p-toluenesulphonic acid were added, followed by dropwise addition of 6.35 g (75.6 mmol) of dihydropyran. The solution was warmed to 20°, stirred for 18 hr, and then extracted with saturated aqueous NaHCO3 (25 mL) and brine (25 mL). The solution was dried (MgSO4), concentrated in vacuo, and distilled, yielding 12.96 g of 6 (96% yield).

WORKUP

后处理

  1. temperaturecooled to 0°
  2. temperatureThe solution was warmed to 20°
  3. extractionextracted with saturated aqueous NaHCO3 (25 mL) and brine (25 mL)
  4. dry with materialThe solution was dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. distillationdistilled