HRID1112108

反应详情

EQUATION

反应方程式

HRID 1112108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 10 g. (0.064 mole) of 3-mercapto-4-n-butyl-1,2,4-triazole and 2.6 g. (0.064 mole) of sodium hydroxide in 200 ml. of methanol was added 9.9 g. (0.064 mole) of p-methoxybenzyl chloride. The reaction mixture was heated at reflux about 20 hours. The solvent was evaporated off, the residue washed with water, dried and distilled. There was obtained 17.8 g. of yellow liquid distilling at 190°-205° C. at 0.03 mm. Nuclear magnetic resonance and ultraviolet spectra indicated this to be approximately an equal mixture of 3-(4-methoxybenzylmercapto)-4-n-butyl-1,2,4-triazole and 4-n-butyl-2-(4-methoxybenzyl)-1,2,4-triazoline-3-thione.

WORKUP

后处理

  1. additionTo a mixture of 10 g
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux about 20 hours
  4. customThe solvent was evaporated off
  5. washthe residue washed with water
  6. customdried
  7. distillationdistilled
  8. customThere was obtained 17.8 g
  9. distillationof yellow liquid distilling at 190°-205° C. at 0.03 mm
  10. additionan equal mixture of 3-(4-methoxybenzylmercapto)-4-n-butyl-1,2,4-triazole and 4-n-butyl-2-(4-methoxybenzyl)-1,2,4-triazoline-3-thione