Reaktion #2178222

Reaktionsgleichung

1-(5-fluoro-2-hydroxyphenyl)ethanone

methyl bromoacetate

potassium carbonate

→

compound

Ausbeute 58.0%

methyl 5-fluoro-3-methyl-1-benzofuran-2-carboxylate

Ausbeute 58.0%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe insoluble material was filtered off
2. 2
   workup.ADDITION1,8-diazabicyclo[5.4.0]undec-7-ene (97.1 mL) was added
3. 3
   workup.STIRRINGthe mixture was stirred at 120° C. for 30 min
4. 4
   workup.ADDITION1N Hydrochloric acid was added to the reaction mixture at 0° C.
5. 5
   Filtrationthe resulting precipitate was collected by filtration

Vorschrift

To a mixture of 1-(5-fluoro-2-hydroxyphenyl)ethanone (100 g), methyl bromoacetate (67.6 mL) and N,N-dimethylformamide (500 mL) was added potassium carbonate (135 g), and the mixture was stirred at 50° C. for 2 hr. The insoluble material was filtered off, 1,8-diazabicyclo[5.4.0]undec-7-ene (97.1 mL) was added, and the mixture was stirred at 120° C. for 30 min. 1N Hydrochloric acid was added to the reaction mixture at 0° C., and the resulting precipitate was collected by filtration to give the title object compound (77.9 g, 58%) as a white solid.

Quelle