1-methoxy-1-methyl-3-phenylurea synthesis
- Product Name:1-methoxy-1-methyl-3-phenylurea
- CAS Number:1576-17-6
- Molecular formula:C9H12N2O2
- Molecular Weight:180.2
Yield:1576-17-6 95.1%
Reaction Conditions:
with 18-crown-6 ether;sodium hydroxide in 5,5-dimethyl-1,3-cyclohexadiene;water at 20 - 75;Temperature;Solvent;
Steps:
2.3 synthesis of 1-methoxy-1-methyl-3-phenylurea
In a 1000 ml flask add obtained in preparation 230 g 1-hydroxy-3-phenylurea, plus xylene 400 ml, sulfuric acid dimethyl ester 500 g and 18-crown-6 catalyst of 0.5 g. In the 20 °C -40 ° C dropping between 30% NaOH aqueous solution 360g , dropping time is 0.5 - 1 hour, heating to 65 °C -75 °C, layering, eliminating water layer, organic layer then adding 400 ml clear water to wash, the layering. Organic layer cooling to 0 °C -10 ° C crystallization, filtration. The filter cake 52 °C left and right vacuum drying. Product 1-methyl-1-methoxy-phenylurea 255 g. Product melting point 58.7 °C, content of 99.1%. The product yield 95.1% (in order to 1-hydroxy-3-phenyl ureometer ).
References:
CN103910654,2016,B Location in patent:Paragraph 0015; 0016; 0026; 0032; 0033; 0040; 0041
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