HRID576622

反应详情

EQUATION

反应方程式

HRID 576622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of aqueous hydrobromic acid (16 mL, 48% solution in water), propionic acid (2.8 mL) and phenol (2 g) was added 5-bromo-2-(p-tolylsulfonyl)isoindoline (2.4 g, 6.8 mmol). The resulting mixture was heated to reflux and stirred at this temperature for 10 hr then cooled to room temperature. This mixture was diluted with water (20 mL) and extracted with ether (2×50 mL). The aqueous extract was brought to pH 14 with 5M sodium hydroxide solution. This solution was extracted with ether (3×). The ether extract is washed with brine, dried over magnesium sulfate, and concentrated to give the title compound as an oil.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux
  3. extractionextracted with ether (2×50 mL)
  4. extractionThe aqueous extract
  5. extractionThis solution was extracted with ether (3×)
  6. extractionThe ether extract
  7. washis washed with brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated