• 专利标题:   Preparing dimethylcarbamoyl chloride useful as key intermediate in preparing pirimicarb and triazamate pesticides, comprises e.g. reacting N-chloro-N-methylmethanamine under carbon monoxide gas in presence of palladium-nickel/graphene oxide.
  • 专利号:   CN112778161-A
  • 发明人:   CHENG W, SHOU W, LIU C, SHEN L, ZHU Z, CAO J
  • 专利权人:   ANHUI GUANGXIN AGROCHEMCIAL CO LTD
  • 国际专利分类:   C07C269/04, C07C271/04
  • 专利详细信息:   CN112778161-A 11 May 2021 C07C-269/04 202149 Pages: 8 Chinese
  • 申请详细信息:   CN112778161-A CN10051783 14 Jan 2021
  • 优先权号:   CN10051783

▎ 摘  要

NOVELTY - Preparing dimethylcarbamoyl chloride (I), comprises adding N-chloro-N-methylmethanamine (II) and catalyst into a reactor, introducing carbon monoxide gas, heating it at 50-100 degrees C, and controlling the internal pressure of the reactor at 1-10 bar to obtain final product, where the addition amount of (II) is 1-100 g/minute, and the catalyst is palladium-nickel/graphene oxide. The catalyst is prepared by mixing 50 ml deionized water, 0.5 ml of 0.02 mol/l palladium(II) chloride, 0.5 ml of 0.02 mol/l nickel(II) chloride and 0.8 g graphene oxide, fully dissolving the mixture, ultrasonic treating at room temperature under ultrasonic powers of 160 W for 30 minutes, adding 2 ml hydrazine hydrate dropwise, and continuously ultrasonic treating at 60 degrees C under ultrasonic powers of 160 W for 1 hours, centrifuging, washing with deionized water for 3 times, centrifuging and separating, and vacuum drying. USE - (I) is useful as key intermediate in preparing pirimicarb and triazamate pesticides. ADVANTAGE - The method: is high-efficient and environmentally friendly. DETAILED DESCRIPTION - Preparing dimethylcarbamoyl chloride of formula ((CH3)2N-C(=O)-Cl) (I), comprises adding N-chloro-N-methylmethanamine of formula ((CH3)2N-Cl) (II) and catalyst into a reactor, introducing carbon monoxide gas, heating it at 50-100 degrees C, and controlling the internal pressure of the reactor at 1-10 bar to obtain final product, where the addition amount of (II) is 1-100 g/minute, and the catalyst is palladium-nickel/graphene oxide. The catalyst is prepared by mixing 50 ml deionized water, 0.5 ml of 0.02 mol/l palladium(II) chloride, 0.5 ml of 0.02 mol/l nickel(II) chloride and 0.8 g graphene oxide, fully dissolving the mixture, ultrasonic treating at room temperature under ultrasonic powers of 160 W for 30 minutes, adding 2 ml hydrazine hydrate dropwise, and continuously ultrasonic treating at 60 degrees C under ultrasonic powers of 160 W for 1 hours, centrifuging, washing with deionized water for 3 times, centrifuging and separating, and vacuum drying. The reactor is device has fed pipeline 1 provided with dimethylamine chloride, catalyst bed 3, and fed pipeline 2 provided with carbon monoxide, where the liquid phase product is introduced in a rectification tower through pipeline 4 for refining, the refined product obtained in pipeline 6 is condensed to obtain refined dimethylcarbamoyl chloride, and the by-product is discharged through pipeline 7.