HRID322852

反应详情

EQUATION

反应方程式

HRID 322852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2,4-dibenzyloxybenzonitrile (1.89 g) in dry toluene (200 mL) is treated with trimethyltin chloride (6 g) and sodium azide (2 g). The mixture is stirred at reflux for 3 days, evaporated and the residue partitioned between dichloromethane (250 mL) and water (165 mL). The organic phase is washed with brine (165 mL), dried over magnesium sulphate and evaporated. The resulting semi-solid is triturated with ether (30 mL) and the solid washed with pentane and crystallised from a mixture of ethyl acetate and pentane to give 5-(2,4-dibenzyloxyphenyl)-2H-tetrazole hydrate (1.55 g) as a white solid, m.p. 178-179° C. [Elemental analysis:- C,69.7; H,5.02; N,15.4%. Calculated for C21H18N4O2.0.2H2O:- C,68.68; H,5.12; N,15.48%].

WORKUP

后处理

  1. temperatureat reflux for 3 days
  2. customevaporated
  3. customthe residue partitioned between dichloromethane (250 mL) and water (165 mL)
  4. washThe organic phase is washed with brine (165 mL)
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe resulting semi-solid is triturated with ether (30 mL)
  8. washthe solid washed with pentane
  9. customcrystallised from a mixture of ethyl acetate and pentane