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4-Chloro-2-(1-piperidinyl)quinazoline, 97% synthesis

6synthesis methods
-

Yield:134962-82-6 72%

Reaction Conditions:

in 1,4-dioxane at 150; for 0.0833333 h;Microwave irradiation;

Steps:

1.3

2,4-Dichloroquinazoline (1.5 g, 7.5 mmol) was dissolved in 1,4-dioxane (15 mL). N-Methylpiperidine (961 L, 7.9 mmol) was added and the mixture was heated to 150° C. for 5 min under microwave irradiation. The mixture was diluted with EtOAc and washed with saturated aqueous NaHCO3 and brine (×2). The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The crude product was purified by column chromatography (5% EtOAc-petrol) to afford the title compound as a yellow oil that solidified on evaporation from petrol to a yellow solid (1.33 g, 72%).1H NMR (DMSO): 7.95-7.91 (1H, m), 7.77 (1H, ddd, J 8.5, 7.0 and 1.4), 7.54-7.49 (1H, m), 7.32 (1H, ddd, J 8.1, 7.0 and 1.1), 3.84-3.79 (4H, m) and 1.69-1.51 (6H, m).

References:

US2010/317607,2010,A1 Location in patent:Page/Page column 24