HRID440652

反应详情

EQUATION

反应方程式

HRID 440652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 20.0 g (0.088 mole) of 3-chloro-2-(2-methyl-2-propen-1-yl)-6-nitrophenol and 0.35 g (0.002 mole) of p-toluenesulfonic acid in 100 mL of xylene was heated at reflux for approximately 16 hours. The solvent was evaporated under reduced pressure, leaving a residue which was passed through a column of silica gel, eluting with methylene chloride. The product-containing fractions were combined, washed with an aqueous solution of sodium hydroxide, dried over anhydrous magnesium sulfate, and the solvent evaporated under reduced pressure, yielding 16.85 g of 4-chloro-2,3-dihydro-2,2-dimethyl-7-nitrobenzofuran as an oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for approximately 16 hours
  3. customThe solvent was evaporated under reduced pressure
  4. customleaving a residue which
  5. washeluting with methylene chloride
  6. washwashed with an aqueous solution of sodium hydroxide
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent evaporated under reduced pressure