• 专利标题:   Catalyst composition useful for catalyzing methylation and/or propargylation reactions, and preparing pyraclonil, comprises e.g. graphene oxide and anion exchange resin, sodium bromide, potassium bromide, copper chloride, tetrabutylamine bromide, and tetrabutylamine iodide.
  • 专利号:   CN114453027-A
  • 发明人:   KONG F, CHEN L, SU W, SUN Y, ZHANG K, ZENG R
  • 专利权人:   JIANGSU AGROCHEM LAB CO LTD, UNIV SOOCHOW
  • 国际专利分类:   B01J021/18, B01J027/08, B01J027/122, B01J029/70, B01J031/02, B01J031/04, B01J031/06, B01J031/08, B01J031/30, B01J035/00, C07D471/04
  • 专利详细信息:   CN114453027-A 10 May 2022 B01J-031/30 202286 Chinese
  • 申请详细信息:   CN114453027-A CN11555818 17 Dec 2021
  • 优先权号:   CN11555818

▎ 摘  要

NOVELTY - Catalyst composition, comprises 50-60 pts. wt. 4 A molecular sieve, graphene oxide and anion exchange resin as first composite component, 20-30 pts. wt. sodium bromide, potassium bromide, copper chloride, copper bromide, sodium iodide, potassium iodide, copper iodide, cuprous iodide and/or copper acetate as second composite component, and 10-15 pts. wt. triethylbenzylamine chloride, tetrabutylamine bromide, tetrabutylamine iodide, PEG-400, PEG-600 and/or 18-crown-6 as third composite component. USE - The composition is useful for catalyzing methylation and/or propargylation reactions, and preparing pyraclonil (all claimed). ADVANTAGE - The composition utilizes readily available raw materials; has high product yield, low production cost, and mild reaction conditions, and is environmentally friendly. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is also included for preparing pyraclonil comprising (i) reacting 5-amino-1-(3-chloro-4,5,6,7-tetrahydropyrazolo1,5-apyridin-2-yl)-1H-pyrazole-4-carbonitrile with paraformaldehyde and sodium alkoxide in the first solvent organic solvent at 15-20 ℃ under the action of the first catalyst composition, adding reducing agent into reaction system to carry out reduction reaction to obtain 1-(3-chloro-4,5,6,7-tetrahydropyrazolo1,5-apyridin-2-yl)-5-(methylamino)-1H-pyrazole-4-carbonitrile, (ii) reacting 1-(3-chloro-4,5,6,7-tetrahydropyrazolo1,5-apyridin-2-yl)-5-(methylamino)-1H-pyrazole-4-carbonitrile with chloropropyne under the action of the second catalyst composition at 25-60 ℃ in the second organic solvent to which a basic substance is added to obtain 1-(3-chloro-4,5,6,7-tetrahydropyrazolo1,5-apyridin-2-yl)-5-(methyl(prop-2-ynyl)amino)-1H-pyrazole-4-carbonitrile.