ChemicalBook CAS DataBase List 4-Nitrobenzyl 2-diazoacetoacetate

4-Nitrobenzyl 2-diazoacetoacetate synthesis

8synthesis methods

Product Name:4-Nitrobenzyl 2-diazoacetoacetate
CAS Number:82551-63-1
Molecular formula:C11H9N3O5
Molecular Weight:263.21

The invention presents a method for preparing p-nitrobenzyl 2-diazoacetoacetate through a two-step reaction process. This method offers numerous benefits, such as streamlined processing steps, easier industrial production, reduced production costs, enhanced product quality, and increased yield. Using nitrobenzyl alcohol as a standard, the overall mol yield achieves 95% or more, and the purity of the product compound (IV) reaches at least 99.5%.
CN101983958A/en

619-73-8 Synthesis

619-73-8
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2009-97-4
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82551-63-1
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Yield:82551-63-1 97.1%

Reaction Conditions:

with sodium ethanolate in toluene at 0; for 6.5 h;Reflux;Reagent/catalyst;Solvent;Temperature;

Steps:

1 Example 1

In a 3000 ml reaction flask with a fractionation apparatus, 275.7 g (1.8 mol) of p-nitrobenzyl alcohol,337.3 g (2.16 mol) of 2-diazo acetoacetate,2.8g of sodium ethoxide and 1380g of toluene are warmed up to reflux, and the ethanol fraction is slowly collected. After 5.5 hours of reaction, the temperature is reduced to 0-10°C, and the temperature is stirred for 1 hour.Filtration and drying of 2-diazoacetoacetic acid p-nitrobenzyl ester product460 g, yield 97.1%, HPLC: 99.8%.

References:

CN107556212,2018,A Location in patent:Paragraph 0029-0030; 0031-0036; 0037-0044

61312-84-3 Synthesis