Reaktion #648219

Reaktionsgleichung

pyridinium p-toluenesulfonate

1-{2-[5-fluoro-4-(7-{2-fluoro-5-[2-(tetrahydro-pyran-2-yloxy)-ethoxy]-pyridin-4-yl}-benzo[b]thiophen-2-yl)-pyrimidin-2-ylamino]-ethyl}-imidazolidin-2-one

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title compound

Ausbeute 87.0%

1-[2-(5-Fluoro-4-{7-[2-fluoro-5-(2-hydroxyethoxy)pyridin-4-yl]benzo[b]thiophen-2-yl}pyrimidin-2-ylamino)ethyl]imidazolidin-2-one

Ausbeute 87.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturCool the solution
2. 2
   EinengenConcentrate the solution in vacuo to yellow oil
3. 3
   SonstigePurify the oil by column chromatography (methylene chloride to 10% methanol in methylene chloride)

Vorschrift

Add pyridinium p-toluenesulfonate (4.3 mg, 0.02 mmol) to a solution of 1-{2-[5-fluoro-4-(7-{2-fluoro-5-[2-(tetrahydro-pyran-2-yloxy)-ethoxy]-pyridin-4-yl}-benzo[b]thiophen-2-yl)-pyrimidin-2-ylamino]-ethyl}-imidazolidin-2-one (100 mg, 0.17 mmol) in ethanol (4 mL). Stir the mixture at 55° C. overnight. Cool the solution. Concentrate the solution in vacuo to yellow oil. Purify the oil by column chromatography (methylene chloride to 10% methanol in methylene chloride) to afford the title compound (75 mg, 87%) as a light yellow solid. MS (ES) m/z 513 [M+1]+.

Quelle