PIRIMICARB-DESAMIDO synthesis
- Product Name:PIRIMICARB-DESAMIDO
- CAS Number:40778-16-3
- Molecular formula:C8H13N3O
- Molecular Weight:167.21
17094-21-2
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311-77-3
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40778-16-3
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Yield:40778-16-3 95.3%
Reaction Conditions:
Stage #1: 1,1-dimethylguanidine dihydrogensulfatewith sodium hydroxide in methanol at 35; for 2 h;
Stage #2: 2-methyl-acetoacetic acid methyl ester in methanol at 105;Inert atmosphere;Dean-Stark;
Steps:
11 Synthesis of 2,2-Dimethylamino-5,6-Dimethyl-4-hydroxypyrimidine
In a 500ml three-necked reaction flask equipped with stirring, thermometer and condenser, Add 89.8g (0.33mol) metformin sulfate, 24.0g (0.6mol) sodium hydroxide and 150g methanol, Stir at 35°C for 2 hours, filter, and transfer the filtrate to a stirrer, thermometer, In the 500ml four-necked reaction flask of the condenser, desolventize. After desolventization is completed, The reaction flask is equipped with a water separator, and 129.6g (0.9mol) methyl α-methylacetoacetate is added, A nitrogen carrier gas was introduced at a flow rate of 20ml/min, the temperature was raised to 105°C, and water and methanol were separated. When completely anhydrous and methanol are separated, the temperature is reduced to 70°C, 129.6g petroleum ether is added, After stirring and cooling, filter, wash the filter cake twice with 89.8g water, The dried product is 2,2-dimethylamino-5,6-dimethyl-4-hydroxypyrimidine, the yield is 95.3%, and the content is 98.0%.
References:
CN111978262,2020,A Location in patent:Paragraph 0078-0080
19810-73-2
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40778-16-3
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17094-21-2
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6145-42-2
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40778-16-3
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