Reaktion #527745

Reaktionsgleichung

N-{{5-[(2-chloro-α,α,α-trifluoro-p-tolyl)oxy]-2-nitrophenyl}carbamoyl}glycine ethyl ester

N-(chlorocarbonyl) isocyanate

N-(chlorocarbonyl) isocyanate

→

title product

Ethyl 3-{5-[(2-chloro-α,α,α-trifluoro-p-tolyl)oxy]-2-nitrophenyl}tetrahydro-2,4,6-trioxo-s-triazine-1(2H)-acetate

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated at 60° C. for 4 hours
2. 2
   Temperaturcooled to room temperature
3. 3
   Filtrationfiltered
4. 4
   Sonstigeto obtain a solid
5. 5
   WaschenThe solid is washed with petroleum ether
6. 6
   Sonstigedried

Vorschrift

A mixture of N-{{5-[(2-chloro-α,α,α-trifluoro-p-tolyl)oxy]-2-nitrophenyl}carbamoyl}glycine ethyl ester (75.0 g, 0.162 mol) and N-(chlorocarbonyl) isocyanate (35.0 g, 0.332 mol) in toluene is heated at 60° C. overnight, treated with additional N-(chlorocarbonyl) isocyanate (4.25 g), heated at 60° C. for 4 hours, cooled to room temperature and filtered to obtain a solid. The solid is washed with petroleum ether and dried to give the title product as a white solid which is identified by 1H and 13CNMR spectral analyses.

Quelle