Reaction #1519104

Reaction equation

6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol

1-methyl-piperazine

→

6-[4-(4-Methyl-piperazin-1-yl)-pyrid-2-yl]-2-pyrid-2-yl-pyrimidin-4-ol

Solvents

2-methyl-2-butanol

Conditions

Workup

1. 1
   Temperatureis refluxed for 22 hours
2. 2
   Concentrationconcentrated to dryness
3. 3
   Othera rotary evaporator
4. 4
   workup.ADDITION50 ml of water are added
5. 5
   workup.ADDITION3.6 g of EDTA are added
6. 6
   ExtractionExtraction
7. 7
   Dryingdried (sodium sulfate)
8. 8
   ConcentrationConcentration
9. 9
   Othera rotary evaporator
10. 10
    Otherthe crude product is recrystallised from toluene

Procedure

A mixture of 3.51 g (12.3 mmol) of 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol, 27.4 ml (303 mmol, 20 equivalents, 30.38 g) of 1-methyl-piperazine and 84 mg (0.05 mmol, 0.05 equivalent) of zinc(II) chloride in 50 ml of 2-methyl-2-butanol is refluxed for 22 hours and concentrated to dryness using a rotary evaporator. 50 ml of water are added, 3.6 g of EDTA are added, and the pH is adjusted to 9 using dilute sodium hydroxide solution. Extraction is carried out three times using 150 ml of chloroform each time, and the organic extracts are combined and dried (sodium sulfate). Concentration is carried out using a rotary evaporator and the crude product is recrystallised from toluene. 6-[4-(4-Methyl-piperazin-1-yl)-pyrid-2-yl]-2-pyrid-2-yl-pyrimidin-4-ol is obtained in the form of a whitish solid.

Source