Reaktion #6999

Reaktionsgleichung

2-methoxyphenol

N,N-dimethylaniline

phosgene

DMF

→

2-methoxyphenyl chloroformate

Ausbeute 50.0%

Lösungsmittel

toluene

chlorobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic layer was separated
2. 2
   Einengenconcentrated in vacuo
3. 3
   workup.DISTILLATIONThe residue was distilled (Buchi Kugelrohr; bp=115° C. @ 10 mm Hg)

Vorschrift

A solution of 2-methoxyphenol (2 g, 16.1 mmol), N,N-dimethylaniline (1.95 g, 16.1 mmol), phosgene (8.34 mL of a 1.93 M solution in toluene, 16.1 mmol) and a catalytic amount of DMF in chlorobenzene (5 mL) was stirred in a pressure tube for 2 h at 80° C. The organic layer was separated and concentrated in vacuo. The residue was distilled (Buchi Kugelrohr; bp=115° C. @ 10 mm Hg) to provide 2-methoxyphenyl chloroformate (1.5g; 50%) as a clear oil.

Quelle