DIMETHIRIMOL synthesis
- Product Name:DIMETHIRIMOL
- CAS Number:5221-53-4
- Molecular formula:C11H19N3O
- Molecular Weight:209.29
Yield:5221-53-4 98.1%
Reaction Conditions:
Stage #1:1,1-dimethylguanidine dihydrogensulfate with sodium hydroxide in methanol at 60; for 1 h;
Stage #2:methyl α-butylacetoacetate in methanol at 105;Inert atmosphere;Dean-Stark;Temperature;
Steps:
1-9 Synthesis of 2,2-Dimethylamino-5-n-butyl-6-methyl-4-hydroxypyrimidine
In a 500ml three-necked reaction flask equipped with stirring, thermometer and condenser, Add 89.8g (0.33mol) N,N-dimethylguanidine sulfate, 24.0g (0.6mol) sodium hydroxide and 150g methanol, Stir at 60°C for 1 hour, filter, and transfer the filtrate to a stirred, In a 500ml four-necked reaction flask with thermometer and condenser, After desolvation is completed, the reaction flask is equipped with a water separator, Add 258.0g (1.5mol) of methyl α-butylacetoacetate, and introduce nitrogen carrier gas at a flow rate of 20ml/min, Raise the temperature to 105°C, separate water and methanol, and when completely anhydrous and methanol separate, Cool down to 70°C, add 258.0g petroleum ether, stir to cool down, filter, and wash the filter cake twice with 89.8g water. The dried product is 2,2-dimethylamino-5-n-butyl-6-methyl-4-hydroxypyrimidine, Yield The yield is 98.1%, and the content is 98.1%.
References:
Xi'an Modern Chemical Institute;Chen Tao;Yang Cuifeng;Rong Haojie;Su Tianduo;Xu Zegang CN111978262, 2020, A Location in patent:Paragraph 0048-0074