Reaktion #61665

Reaktionsgleichung

trichloromethylchloroformate

2-methoxy-6-nitro-phenylamine

THF

→

ethyl (2-methoxy-6-nitro-phenyl)-carbamate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONThe solvent is distilled off
2. 2
   workup.STIRRINGthe residue is stirred with isopropanol, during which time a yellow solid
3. 3
   Sonstigeis precipitated

Vorschrift

17.1 mL (0.141 mol) trichloromethylchloroformate are added dropwise at reflux temperature to a solution of 23.8 g (0.142 mol) 2-methoxy-6-nitro-phenylamine in 300 mL THF and then the mixture is stirred for 4 hours at this temperature. The solvent is distilled off and the residue is stirred with isopropanol, during which time a yellow solid is precipitated. Yield: 25.0 g (73%); mass spectroscopy: [M+H]+=241.

Quelle