Reaktion #164242

Reaktionsgleichung

aluminum trichloride

methyl 2-chloro-2-oxoacetate

2-methylthiophene

→

oil

Ausbeute 99.8%

(5-methyl-thiophen-2-yl)-oxo-acetic acid methyl ester

Ausbeute 99.8%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThen the mixture is cooled at 0° C.
2. 2
   Waschenthe organic phase is washed with aq. NaHCO3 and brine
3. 3
   Trocknendried over Na2SO4
4. 4
   Sonstigeevaporated

Vorschrift

To a suspension of aluminum trichloride (2.75 g, 20.6 mmol) and methyl 2-chloro-2-oxoacetate (1.90 mL, 20.7 mmol) in dry DCM (25 mL), cooled at 0° C. and under nitrogen atmosphere, is added 2-methylthiophene (1.00 mL, 10.33 mmol) dropwise. The reaction is stirred at RT for 15 hours. Then the mixture is cooled at 0° C., ice-water is slowly added and the organic phase is washed with aq. NaHCO3 and brine, dried over Na2SO4 and evaporated to obtain intermediate I266 as a brown oil (1.9 g, quantitative yield).

Quelle