Reaktion #5453

Reaktionsgleichung

methyl iodide

ethyl 2,3,4,5-tetrafluorobenzoylacetate

carbon disulfide

triethylamine

→

title compound

Ausbeute 74.0%

3-Ethoxycarbonyl-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

Ausbeute 74.0%

Lösungsmittel

dimethyl sulfoxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred for 2 hours
2. 2
   FiltrationThe crystals deposited were collected by filtration
3. 3
   Sonstigedried

Vorschrift

To a solution of 3.00 g (11.4 mmol) of ethyl 2,3,4,5-tetrafluorobenzoylacetate, 870 mg (11.4 mmol) of carbon disulfide and 9 ml of dried dimethyl sulfoxide were added 2.31 g (22.8 mmol) of triethylamine at room temperature, and the mixture was stirred for 1 hour at room temperature. Then, at room temperature, 3.24 g (22.8 mmol) of methyl iodide were added and the mixture was stirred for 2 hours, which was poured into ice-water. The crystals deposited were collected by filtration and dried to obtain 2.81 g (8.41 mmol) of title compound (yield 74%.

Quelle