4-Nitrobenzyl 2-diazoacetoacetate synthesis
- Product Name:4-Nitrobenzyl 2-diazoacetoacetate
- CAS Number:82551-63-1
- Molecular formula:C11H9N3O5
- Molecular Weight:263.21
CN101983958A/en
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
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