Reaktion #49764

Reaktionsgleichung

hydrochloric acid

2-Fluoro-4-chloro-5-methoxycarbonyloxyaniline

potassium carbonate

benzyl chloroformate

→

benzyl N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)carbamate

Ausbeute 91.1%

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated for 2 hours
2. 2
   Temperaturwhile refluxing
3. 3
   SonstigeAfter completion of the reaction
4. 4
   Extraktionextracted with ethyl acetate (50 ml×3)
5. 5
   SonstigeAfter drying
6. 6
   Einengenthe organic layer was concentrated

Vorschrift

2-Fluoro-4-chloro-5-methoxycarbonyloxyaniline (2.00 g, 6.86 mmol), potassium carbonate (1.42 g, 10.3 mmol), benzyl chloroformate (1.17 g, 6.86 mmol) and acetone (20 ml) as a solvent were charged into a 100 cc two-necked flask, and heated for 2 hours while refluxing. After completion of the reaction, the mixture was added to 1H hydrochloric acid (50 ml), and extracted with ethyl acetate (50 ml×3). After drying, the organic layer was concentrated to obtain substantially pure benzyl N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)carbamate as a solid (2.21 g, 91.1% yield).

Quelle