Potassium Carbonate → HCID 28254339, Verbindung

In a 30 mL large microwave vial, 2-chloro-5-nitropyridine (1.041 g, 6.57 mmol, 1 equiv) was dissolved in 5.5 mL of dimethylformamide. 3-(1-methylethyl)phenol (0.90 mL, 6.57 mmol, 1 equiv) and potassium carbonate (4.54 g, 32.8 mmol, 5 equiv) were added. The reaction mixture was heated under microwave irradiation for 1 hour at 110° C. (Biotage Initiator). The reaction mixture was filtered. The filtrated solid was washed with dichloromethane (30 mL). The volatiles were evaporated under vacuum. The crude compound was dissolved in dichloromethane (20 mL) and brine was added (20 mL). The compound was extracted 2 times with dichloromethane (2×20 mL) and 2 times with ethyl acetate (2×20 mL). The organic phase was dried over sodium sulphate. Evaporation afforded the title compound (1.402 g).

1. filtrationThe reaction mixture was filtered
2. washThe filtrated solid was washed with dichloromethane (30 mL)
3. customThe volatiles were evaporated under vacuum
4. dissolutionThe crude compound was dissolved in dichloromethane (20 mL)
5. additionbrine was added (20 mL)
6. extractionThe compound was extracted 2 times with dichloromethane (2×20 mL) and 2 times with ethyl acetate (2×20 mL)
7. dry with materialThe organic phase was dried over sodium sulphate
8. customEvaporation

ORD-Eintrag

ord-757a8a6bd468494db0dbf95ad060d823

Quelldatensatz

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09216967B2