2-chloro-5-[[(2Z)-2-(nitromethylidene)imidazolidin-1-yl]methyl]pyridine synthesis
- Product Name:2-chloro-5-[[(2Z)-2-(nitromethylidene)imidazolidin-1-yl]methyl]pyridine
- CAS Number:101336-63-4
- Molecular formula:C10H11ClN4O2
- Molecular Weight:0
70258-18-3
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Yield:101336-63-4 86%
Reaction Conditions:
Stage #1: 1,1-dichloro-2-nitro ethylenewith sodium methylate in iso-butanol; for 5 h;Reflux;
Stage #2: ethylenediamine in iso-butanol; for 6 h;Reflux;
Stage #3: 2-chloro-5-(chloromethyl)pyridinewith tetrabutylammomium bromide;sodium hydroxide in iso-butanol at 25; for 5 h;Reagent/catalyst;Solvent;
Steps:
1-5 Example 1
In a 250 ml three-necked flask were added nitrodichloroethylene (28.2 g, 0.2 mol) and 50 mL of sec-butanol, and sodium methoxide solid (21.6 g, 0.4 mol) was added, and the temperature was raised to reflux.After 5 h of reaction, cool to room temperature, add anhydrous ethylenediamine (11.4 g, 0.19 mol), and continue refluxing for 6 h.Cool to room temperature, add tetrabutylammonium bromide (3.22g, 10mmol), sodium hydroxide (12.0g, 0.3mol), 2-chloro-5-chloromethylpyridine (29.0g, 0.18mol), and stir at 25 ° C for 5h Rear,Suction filtration, the filter cake was recrystallized from absolute ethanol, and dried to obtain clopyridinenitromethyleneimidazolidine (white solid, melting point: 158.4-160.8 ° C). The liquid phase content was 98% and the yield was 86% (based on nitrodichloroethylene).
References:
CN104447690,2019,B Location in patent:Paragraph 0021-0031
