4-Methylphenylsulfonylurea synthesis
- Product Name:4-Methylphenylsulfonylurea
- CAS Number:1694-06-0
- Molecular formula:C8H10N2O3S
- Molecular Weight:214.24
4083-64-1
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1694-06-0
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Yield:1694-06-0 96.3%
Reaction Conditions:
with ammonia in toluene at -5 - 5; under 4500.45 Torr; for 4 h;Inert atmosphere;Large scale;
Steps:
1-4 A simple preparation method of p-toluenesulfonylurea includes the following steps
First fill the 3000L stainless steel reactor with nitrogen to replace the air in it.Then add p-toluenesulfonyl isocyanate (Sinopec Group Chemical Reagent Co., Ltd.) (197kg, 1000mol) and toluene (1000L),Stir down the temperature to -5 to 5 ° C, and slowly fill in ammonia gas (136kg, 8000mol, about 0.6MPa).A white solid precipitated during the 4 h incubation reaction.Slowly vent (absorbed with 1% hydrochloric acid solution), replace with nitrogen, stop refrigeration, slowly raise the temperature to 25-30 ° C, and keep it for 4 hours.Filtration and washing with water to a pH of about 7 gave crude p-toluenesulfonylurea.Then add the crude p-toluenesulfonylurea to a 3000L reactorThen add 2000L of acetonitrile / water (1: 1 by volume), heat to 80 ± 5 , and reflux for 1h.Program to cool down (10 / h), drop below 20 , centrifuge,Dried to give white crystals of p-toluenesulfonylurea (209Kg, yield 96.3%),mp189.5 191.2 ,The purity was 99.9% by HPLC.
References:
Shandong Haiyou Furuida Pharmaceutical Co., Ltd.;Zheng Deqiang;Wei Lekun;Wang Hongchen;Li Xiang;Chen Weibo;Xu Yuelei CN110372545, 2019, A Location in patent:Paragraph 0028-0031; 0036-0047
![hydroxy-[[N-(4-methylphenyl)sulfonylcarbamimidoyl]amino]-oxo-azanium](/CAS/20180529/GIF/5465-99-6.gif)
5465-99-6
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1694-06-0
270 suppliers
$6.00/10g
