Potassium Carbonate → HCID 69224391, Verbindung

Temperatur

200 °C

A mixture of N-(4-tert-butylphenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine 0.173 g, 0.61 mmol), 2,3-dichloropyridine (0.91 g, 0.61 mmol) and potassium carbonate (0.234 g, 1.84 mmol) in DMF was heated in a sealed tube in a microwave (Emrys Optimizer model, Personal Chemistry) at 200° C. for 2 h. The mixture was cooled to r.t. and diluted with water (30 mL). The mixture was extracted with ethyl acetate (3×30 mL). The combined organic extracts were washed with brine, dried over sodium sulfate and concentrated to leave an oil. The product was purified by silica gel chromatography (ethyl acetate/hexane gradient) to obtain 0.035 g of the title compound as a light yellow oil. The oil was dissolved in 1 ml ethyl acetate and treated with 1.0 M HCl in diethyl ether (0.09 mL). The resulting solid was collected by filtration, washed with diethyl ether and dried to give 0.030 g light yellow solid.

1. temperatureThe mixture was cooled to r.t.
2. extractionThe mixture was extracted with ethyl acetate (3×30 mL)
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customto leave an oil
7. customThe product was purified by silica gel chromatography (ethyl acetate/hexane gradient)

ORD-Eintrag

ord-b7aaf726d637453c9928b4f6ec0b9d62

Quelldatensatz

uspto-grants-2008_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07414131B2