It is prepared by the reaction of 2-chloro-2-methyl-propodoxime dimer and sodium methylmercaptan
In the synthesis kettle, industrial ethanol is added, 20% sodium methyl mercaptan is added, heated to 45 ℃, 60 $dimer is added within a certain temperature range, and the heat preservation reaction is carried out for 30 min. Use a vacuum pump to raise the reaction material into a deethanol kettle, and evaporate dilute ethanol under a vacuum of 46 ~ 60kPa. When the liquid temperature reaches 85 ℃ and the temperature is 75 ℃, stop heating and cool the cold water. The material is mentioned in a glass-lined neutralization kettle with a vacuum pump, hydrochloric acid is added dropwise for neutralization when the liquid temperature is lower than 45 ℃, pH = 5~6 is adjusted, the oil layer is placed in a toluene removal kettle, the water layer is placed in an extraction kettle, toluene is extracted with toluene, toluene layer is placed in a toluene removal kettle, toluene is removed under a vacuum of 46~60 kPa.
Isobutyraldehyde method
2-Chloro-2-methylpropanal is dripped into an equal mole of sodium methyl mercaptan under stirring, and the reaction is carried out in an aqueous solution. After the dropwise addition, the water layer is removed and the oil layer is distilled. The obtained 2-methyl-2-methylthiopropanal is a colorless liquid with a boiling point of 140~144 ℃ and a yield of 84.9% ~ 95.2%.
2-methyl -2-methylthiopropanal and 0.5mol hydroxylamine sulfate were stirred and reacted at 80 ℃ for 1h. The reaction was carried out in an aqueous solution. After the reaction was completed, the water layer was removed and the oil layer was distilled under reduced pressure. The obtained 2-methyl -2-methylthiopropanal oxime was a colorless liquid with a boiling point of 76~78 ℃/800Pa and a yield.
Isobutylene method
Isobutene and nitrosyl chloride are reacted in dichloromethane at a molar ratio of 1.1: 1.0 at a temperature of -5~0 ℃. After solvent removal, a dimer with a yield of 66% and a melting point of 104~105 ℃ is obtained. Dissolve this dimer in hot sodium ethoxide ethanol solution, reflux for 5h, remove the solvent and then distill twice to obtain colorless oily propodoxime.