Reacción #327669

Ecuación de reacción

2-Fluoro-5-iodopyridine

1-ethyl-5,5-dimethyl-pyrazolidin-3-one

cesium carbonate

→

1-ethyl-2-(5-iodo-pyridin-2-yl)-5,5-dimethyl-pyrazolidin-3-one

Rendimiento 28.3%

Disolventes

toluene

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe crude product was purified by flash chromatography
2. 2
   Lavadoeluting with an ethyl acetate

Procedimiento

(200 mg, 0.90 mmol) 2-Fluoro-5-iodopyridine was dissolved in toluene (1 ml) and 1-ethyl-5,5-dimethyl-pyrazolidin-3-one [CAS 26485-97-2] (128 mg, 0.90 mmol, 1.0 equiv.) and cesium carbonate (440 mg, 1.35 mmol, 1.5 equiv.) were added under nitrogen. The mixture was stirred for 4 hours at 100° C. The crude product was purified by flash chromatography by directly loading the toluene mixture onto a silica gel column and eluting with an ethyl acetate:heptane gradient 0:100 to 50:50. The desired 1-ethyl-2-(5-iodo-pyridin-2-yl)-5,5-dimethyl-pyrazolidin-3-one (88 mg, 28% yield) was obtained as a yellow oil, MS: m/e=346.3 (M+H+).

Fuente