4-tert-Butyl-2,6-dinitro-3-methoxytoluene synthesis
- Product Name:4-tert-Butyl-2,6-dinitro-3-methoxytoluene
- CAS Number:83-66-9
- Molecular formula:C12H16N2O5
- Molecular Weight:268.27
88-40-4
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83-66-9
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Yield:83-66-9 86%
Reaction Conditions:
with sulfuric acid;nitric acid in dichloromethane at -5; for 0.05 h;Temperature;
Steps:
1.3
100 g of p-tert-butyl-m-methoxytoluene (0.556 mol, 99%)Was dissolved in 200 g (2.33 mol, 99%)Dichloromethane to give a pre-reactant,Pre-cooling spare,300 g of concentrated sulfuric acid (3 mol, 98%)Was dissolved in 600 g of fuming nitric acid (9.05 mol, 95%),Pre-cooling spare,The microreactor cooling system was cooled to -5 ° C,The pre-reactant and mixed acid is injected into the microreactor through a separate valve for nitrification through a parallel flow pump,Control the flow of raw materials 3ml / min,Mixed acid flow of 2.5ml / min,The residence time is 180s, the reaction product is poured into ice water,Separate the organic phase,The aqueous phase is extracted with dichloromethane,The combined organic phase,neutralize,dry,Solvent recovery,Using 3 times the amount of methanol crystallization,129.6 g (99%) of the dried product in vacuo, 86% molar yield.
References:
CN107417537,2017,A Location in patent:Paragraph 0027; 0031; 0036; 0041
108-39-4
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83-66-9
177 suppliers
$50.00/100g
100-84-5
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83-66-9
177 suppliers
$50.00/100g