ChemicalBook CAS DataBase List Metamitron

Metamitron synthesis

5synthesis methods

Product Name:Metamitron
CAS Number:41394-05-2
Molecular formula:C10H10N4O
Molecular Weight:202.21

1603-79-8 Synthesis

1603-79-8
203 suppliers
$7.00/5g

1068-57-1 Synthesis

1068-57-1
388 suppliers
$6.00/5g

41394-05-2
215 suppliers
$16.00/5g

Yield:41394-05-2 92%

Reaction Conditions:

Stage #1:phenylglyoxylic acid ethyl ester;acetic acid hydrazide in ethanol at 25; for 1 h;
Stage #2: with ethylenediaminetetraacetic acid in ethanol at 25; for 3.33333 h;Further stages;Temperature;Concentration;

Steps:

1-10 (Example 1)The method for preparing fentrazone by the one-pot method of this embodiment is specifically as follows:
When equipped with a thermometer,Add 178.18g ethyl benzoylformate (1.0mol) into the 1000mL reaction flask of the reflux condenser,Temperature control 25,Drop 194.5g,40wtpercent acethydrazine in ethanol solution (1.05mol),After about 1h, add 11.7g of EDTA (0.04mol), keep it at 25 and react for 3h.Then add 14.6g of EDTA (0.05mol),After stirring for 20 minutes, a solid precipitated out.Continue to incubate at 25°C for 5h,Sampling control is qualified,Stop the reaction.Then add 147g of ethanol to dilute the reaction solution, then add sodium carbonate to adjust the pH of the reaction solution to 7, and stir for 30 min.Cool the reaction solution of step to 15°C, add 63.8g, 80wtpercent hydrazine hydrate (1.02mol) dropwise for about 1h, keep the temperature at 15°C and react for 7h, the sampling is qualified and stop the reaction.Add 49.2g of anhydrous sodium acetate (0.6mol) and 1.61g of tetrabutylammonium bromide (0.005mol) to the reaction solution of step , stir evenly, and heat to reflux (95±3) for 8h. The sampling is qualified and the reaction is stopped.Slowly lower the temperature of the reaction liquid of step to 0°C, precipitate solids, stir for 30min, and filter with suctionA light yellow solid wet product is obtained,Beat with ice water,Suction filtration,Dry at 60,Get pale yellowcrystalbodyFentrazone186.0g,HPLC purity is 99.2percent,The yield was 92.0percent.

References:

Jiangsu Nongyong Hormone Engineering Technology Research Center Co., Ltd.;Nanjing Gaoheng Biological Technology Co., Ltd.;Jiang Xuming;Zou Peipei;Wei Ping;Sun Yonghui;Kong Fanlei CN111377877, 2020, A Location in patent:Paragraph 0032-0042

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56735-29-6 Synthesis