HRID1391041

反应详情

EQUATION

反应方程式

HRID 1391041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.030 g of p-toluenesulphonic acid and 17.8 g of 3,4-dihydro-2H-pyrane are added to a mixture of 29.8 g of 2,3-dihydroxy-nitrobenzene in 400 ml of absolute benzene and the solution is left to stand for 7 days at 20°. It is filtered through 15 g of a silica gel formulation (Merck silica gel 60; grain size 0.063-0.200 mm) and the silica gel is rinsed with benzene. After distilling off the benzene under reduced pressure, a reddish oil is obtained which, when crystallised from hexane, gives 2-hydroxy-3-(tetrahydropyran-2-yloxy)-nitrobenzene in the form of yellow crystals; melting point 72°-73°.

WORKUP

后处理

  1. waitthe solution is left
  2. filtrationIt is filtered through 15 g of a silica gel formulation (Merck silica gel 60; grain size 0.063-0.200 mm)
  3. washthe silica gel is rinsed with benzene
  4. distillationAfter distilling off the benzene under reduced pressure
  5. customa reddish oil is obtained which, when
  6. customcrystallised from hexane