반응 #1519104

반응 방정식

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

용매

2-methyl-2-butanol

반응 조건

후처리

1. 1
   온도is refluxed for 22 hours
2. 2
   농축concentrated to dryness
3. 3
   기타a rotary evaporator
4. 4
   workup.ADDITION50 ml of water are added
5. 5
   workup.ADDITION3.6 g of EDTA are added
6. 6
   추출Extraction
7. 7
   건조dried (sodium sulfate)
8. 8
   농축Concentration
9. 9
   기타a rotary evaporator
10. 10
    기타the crude product is recrystallised from toluene

실험 절차

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.

출처