1-Methylpiperazine → HCID 178480770, 화합물

HRID 1591579

반응식

HRID 1591579 반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[N:11]=[C:10]([OH:20])[CH:9]=2)[CH:3]=1.[CH3:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>CC(O)(CC)C.[Cl-].[Zn+2].[Cl-]>[CH3:21][N:22]1[CH2:27][CH2:26][N:25]([C:2]2[CH:7]=[CH:6][N:5]=[C:4]([C:8]3[N:13]=[C:12]([C:14]4[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=4)[N:11]=[C:10]([OH:20])[CH:9]=3)[CH:3]=2)[CH2:24][CH2:23]1

참가 물질

5

반응물 2

HCID 531671-MethylpiperazineHCID 1785156306-(4-chloro-2-pyridinyl)-2-pyridin-2-yl-1H-pyrimidin-4-one

생성물 1

HCID 178480770HCID 178480770, 화합물

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 64052-Methyl-2-butanol용매

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.

후처리

  1. temperatureis refluxed for 22 hours
  2. concentrationconcentrated to dryness
  3. customa rotary evaporator
  4. addition50 ml of water are added
  5. addition3.6 g of EDTA are added
  6. extractionExtraction
  7. dry with materialdried (sodium sulfate)
  8. concentrationConcentration
  9. customa rotary evaporator
  10. customthe crude product is recrystallised from toluene

출처 및 근거

ORD 기록
ord-39eba654b162417ca0638b4a13f20a5a
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07291584B2

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