Sodium Carbonate → 2-Chloro-5-(pyridin-2-yl)pyrimidine

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-methyl-5-(2-pyridinyl)-2(1H)pyrimidone (8.994 g, 0.048 mole), phosphorus pentachloride (2.156 g, 0.0104 mole), and phosphorus oxychloride (24 mL) was refluxed at 120° C. for 8 h. POCl3 was distilled out under reduced pressure. The residue was cooled to room temperature and ice-water was added. The mixture was extracted with EtOAc, the organic layer was washed with 15% NaCl solution, brine and dried over MgSO4. Solvent was distilled out under reduced pressure to yield a solid. The water layer was adjusted to pH 6-7 by using saturated Na2CO3, then extracted with EtOAc. The organic layer was washed with 15% NaCl, brine, dried over MgSO4. Solvent was distilled out under reduced pressure to give a solid. After trituration with MeOH, additional product was obtained.

Provenance & Evidence