4,5-DICHLORO-6-METHYLPYRIMIDINE Chemical Properties

Boiling point:

242.6±35.0 °C(Predicted)

Density 

1.404±0.06 g/cm3(Predicted)

storage temp. 

under inert gas (nitrogen or Argon) at 2-8°C

pka

-0.69±0.26(Predicted)

Appearance

Light yellow to yellow Solid-Liquid Mixture

Safety Information

HS Code 

2933599590

4,5-DICHLORO-6-METHYLPYRIMIDINE Usage And Synthesis

Synthesis

2) Preparation of intermediate 4,5-dichloro-6-methylpyrimidine: 50 mL of phosphorus oxychloride (POCl3) was slowly added dropwise to 50 mL of toluene solution containing 14.5 g (0.1 mol) of 5-chloro-6-methylpyrimidin-4(1H)-one. After completion of the dropwise addition, the reaction mixture was heated to reflux for 5-7 hours. The reaction process was monitored by thin layer chromatography (TLC). Upon completion of the reaction, toluene and excess TLC were removed by distillation under reduced pressure. Subsequently, the reaction mixture was carefully poured into ice water. The aqueous phase was extracted with ethyl acetate (3 x 50 mL), the organic phases were combined, dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. Finally, the residue was purified by silica gel column chromatography to afford 14.43 g of the target product 4,5-dichloro-6-methylpyrimidine as a yellow liquid in 88.5% yield.

References

[1] Patent: US2015/225378, 2015, A1. Location in patent: Paragraph 0163; 0164
[2] Patent: EP2913325, 2015, A1. Location in patent: Paragraph 0453; 0454
[3] Patent: CN105348298, 2016, A. Location in patent: Paragraph 0421; 0422; 0423
[4] Patent: CN105732585, 2016, A. Location in patent: Paragraph 0371; 0372; 0373
[5] Patent: CN105777717, 2016, A. Location in patent: Paragraph 0360; 0361; 0362

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