Bispyribac synthesis
- Product Name:Bispyribac
- CAS Number:125401-75-4
- Molecular formula:C19H18N4O8
- Molecular Weight:430.37
303-07-1
113583-35-0
125401-75-4
The general procedure for the synthesis of 2,6-bis((4,6-dimethoxypyrimidin-2-yl)oxy)benzoic acid from 2,6-dihydroxybenzoic acid and 2-methanesulfonyl-4,6-dimethoxypyrimidine was as follows: 0.04 mol of 2,6-dihydroxybenzoic acid, 0.05 mol of 2-methanesulfonyl-4,6-dimethoxypyrimidine, 0.004 mol of tetra butylammonium bromide and 0.08 mol of potassium carbonate in a reaction vessel. 300 mL of toluene was added as a solvent and heated to reflux for 8 to 10 hours. Upon completion of the reaction, the reaction mixture was cooled to room temperature and the solid product was separated by filtration. The filter cake was washed with toluene and subsequently dried. The dried solid product was mixed with 500 mL of water and 30% hydrochloric acid was added slowly and dropwise with stirring to adjust the pH of the system to 3 to 4. It was filtered again and dried to give 15.7 g of the gray solid product 2,6-bis((4,6-dimethoxypyrimidin-2-yl)oxy)benzoic acid with a purity of 97% and a yield of 85%.
303-07-1
465 suppliers
$10.00/5g
113583-35-0
396 suppliers
$6.00/10g
125401-75-4
133 suppliers
$14.00/5g
Yield:125401-75-4 85%
Reaction Conditions:
with tetrabutylammomium bromide;potassium carbonate in tolueneReflux;Reagent/catalyst;Solvent;
Steps:
1
0.04 mol of 2,6-dihydroxybenzoic acid was weighed separately,0.05 mol of 2-methanesulfonyl-4,6-dimethoxypyrimidine,0.004 mol of tetrabutylammonium bromide,0.08 mol of potassium carbonate was placed in a reaction vessel,Add 300mL toluene heated reflux reaction 8 ~ 1 Oh,The reaction is cooled and filtered,The filter cake was washed with toluene,dry,The resulting solid was mixed with 500 mL of water,Stir,Dropping 30% HC1 to the system PH = 3 ~ 4,filter,dry,Was gray and solidbodyBispyribac15.7g,Purity 97%Yield 85%.
References:
Zibo Xinnong Jinongyao Chemical Co.,Ltd;ZHENG, YOUKUI;SONG, JUN;WANG, XIAOWEI CN106083738, 2016, A Location in patent:Paragraph 0019; 0020
2150-45-0
172 suppliers
$5.00/100mg
125401-75-4
133 suppliers
$14.00/5g
303-07-1
465 suppliers
$10.00/5g
125401-75-4
133 suppliers
$14.00/5g