HRID65389

反应详情

EQUATION

反应方程式

HRID 65389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

29.6 g (0.1 mol) of 1-methyl-4-[(2,6-diethylanilino)-acetyl]-thiosemicarbazide were suspended in 150 ml of ethanol and, after adding 7 g of potassium hydroxide in 20 ml of water, the mixture was heated under reflux for 1 hour. Thereafter, most of the solvent was distilled off and 250 ml of water were added to the residue. After acidifying the mixture to pH 5 with glacial acetic acid, the precipitate formed was filtered off and washed thoroughly with water. After drying, 27 g (97% of theory) of 2,6-diethyl-N-[(1-methyl-2-thiono-1,3,4-triazol-5-yl)-methyl]-aniline of melting point 117° to 121° C. were obtained. ##STR88##

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 hour
  3. distillationThereafter, most of the solvent was distilled off
  4. addition250 ml of water were added to the residue
  5. customthe precipitate formed
  6. filtrationwas filtered off
  7. washwashed thoroughly with water
  8. customAfter drying