Reaktion #328421

Reaktionsgleichung

chloroformic acid trichloromethyl ester

4-(4-amino-phenyl)-morpholin-3-one

triethylamine

→

title compound

4-(Isocyanato-phenyl)-morpholin-3-one

Lösungsmittel

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigerose to 35° C
2. 2
   Filtrationwas filtered
3. 3
   Einengenthe filtrate was concentrated in vacuo at 45° C.

Vorschrift

Under an atmosphere of nitrogen to a suspension of 25.9 g of 4-(4-amino-phenyl)-morpholin-3-one (APMO) (MW=192.22; 1 eq.) and 27.2 g of triethylamine (MW=101.19; 2 eq.) in 390 mL of methylene chloride was added at room temperature a solution of 14.6 g chloroformic acid trichloromethyl ester (MW=197.83; 0.55 eq.) in 390 mL of methylene chloride within 10 minutes. The reaction was slight exothermic and the temperature rose to 35° C. After stirring at room temperature for two hours the resulting suspension was filtered and the filtrate was concentrated in vacuo at 45° C. to afford 49.5 g of the title compound. The resulting material was used in the following step without further purification.

Quelle