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ChemicalBook CAS DataBase List Quinclorac

Quinclorac synthesis

6synthesis methods
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Yield:84087-01-4 96.2%

Reaction Conditions:

with hydrogen bromide;manganese (II) acetate tetrahydrate;cobalt(II) diacetate tetrahydrate at 150; under 7500.75 - 12001.2 Torr; for 4.2 h;Concentration;

Steps:

1 preparation of quinchlorac acid

To the volume of 0.5L titanium reactor by adding high-pressure reaction solution,Oxygen into the pressure to l.OMpa,While stirring, the reaction solution was heated to 150 ° C,The pressure rose to 1.6 MPa. The composition of the reaction mixture (i.e., the reaction mixture) was 80.0 g of 7-chloro-8-methylquinoline chloride and 300. Og of acetic acid,5.7 g of cobalt acetate tetrahydrate,1.8 g of manganese acetate tetrahydrate,4.9 g of 40% hydrogen bromide. Reaction 4. lh,The reaction system no longer consumes oxygen,The reaction was terminated. And then discharged to room temperature,The solid product was isolated,dry.getDichloroquinoline acid dry goods75. Og,Content of 86.8%.[0221]75. OgDichloroquinoline acid added to the crude200. Og absolute ethanol,Stirring heated to reflux,Insulation 2h,Cooled to below 10 ° C,filter,Filtrate distillation recovery of ethanol applied,Filter cake drying,TooQuincloracfineProducts63.8 g,Content 97.9%The yield was 96.0%.

References:

CN103420909,2016,B Location in patent:Paragraph 0019; 0020

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