1-Methylpiperazine → HCID 178480770、化合物

HRID 721987

反応式

HRID 721987 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 178480770HCID 178480770、化合物

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 64052-Methyl-2-butanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-62dccb50952a4f20b9d581bd7a6a4f81
出典データセット
uspto-grants-2006_11
特許番号
US07138363B2

関連ノート

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