HRID1606054

反应详情

EQUATION

反应方程式

HRID 1606054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dipropylcarbamoyl chloride (5.5 g.) was added to a solution of 4.4 g. 3-methylsulphonyl-1,2,4-triazole and 6 ml. dry triethylamine in 25 ml. dry tetrahydrofuran and the resulting mixture refluxed for 2.5 hours under anhydrous conditions. The cooled reaction mixture was filtered to remove triethylamine hydrochloride and the filtrate poured with stirring into 150 ml. ice-cold 0.1N aqueous sodium hydroxide. The precipitated product was collected by filtration, washed with ice-cold water, dried, and crystallized twice from toluene to give 1-dipropylcarbamoyl-3-methylsulphonyl-1,2,4-triazole, m.p. 94°C. Elemental analysis satisfactory.

WORKUP

后处理

  1. customThe cooled reaction mixture
  2. filtrationwas filtered
  3. customto remove triethylamine hydrochloride
  4. additionthe filtrate poured
  5. filtrationThe precipitated product was collected by filtration
  6. washwashed with ice-cold water
  7. customdried
  8. customcrystallized twice from toluene