Clomazone synthesis

7synthesis methods

Product Name:Clomazone
CAS Number:81777-89-1
Molecular formula:C12H14ClNO2
Molecular Weight:239.7

611-19-8 Synthesis

611-19-8
455 suppliers
$7.00/25g

81778-07-6
61 suppliers
$61.00/100mg

81777-89-1
224 suppliers
$39.00/50mg

Yield:81777-89-1 973 kg

Reaction Conditions:

with potassium carbonate; pH=7 at 85; for 3 h;Large scale;Reagent/catalyst;

Steps:

1.4; 2.4; 3.4; 4.4 Step four, configuration conversion:
the crude isoxalinone in step 3, first dehydrated under reduced pressure, and then the dried oily mixture is cooled to 45 ° C, then passed through a dry hydrogen chloride gas, and maintained at this temperature for 3 h, Then, 10.5 kg of o-chlorobenzyl chloride, 9.57 kg of 30% by mass of liquid alkali, 2.9 kg of potassium carbonate solid were added to the reaction solution, and the pH was adjusted to 7.00, and then the temperature was raised to 85 ° C for 3 hours, and the amount of o-chlorobenzyl chloride was qualified. After standing, the layers were separated, the lower organic phase was separated, dehydrated under reduced pressure, and the oxaloxone product was distilled off under vacuum, and further purified by petroleum ether to obtain 973 kg of clomazone, content 98.1%. The yield (calculated as hydroxylamine hydrochloride) was 92.1%.

References:

Jiangsu Heben Biochemical Co., Ltd.;Zhejiang Heben Technology Co., Ltd.;Chen Hua;Deng Guiyuan;Jia Lihua;Zeng Ting;Pan Guangfei CN110172042, 2019, A Location in patent:Paragraph 0025; 0028; 0031; 0034; 0037; 0040