1-Methylpiperazine → (2-Chloro-9-cyclopentyl-purin-6-yl)-{2-[3-(4-methyl-piperazin-1-yl)-propoxy]-phenyl}-amine

HRID 1984218Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1984218
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[NH:12][C:13]1[N:21]=[C:20]([Cl:22])[N:19]=[C:18]2[C:14]=1[N:15]=[CH:16][N:17]2[CH:23]1[CH2:27][CH2:26][CH2:25][CH2:24]1.[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1>O>[Cl:22][C:20]1[N:19]=[C:18]2[C:14]([N:15]=[CH:16][N:17]2[CH:23]2[CH2:27][CH2:26][CH2:25][CH2:24]2)=[C:13]([NH:12][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2][N:32]2[CH2:33][CH2:34][N:29]([CH3:28])[CH2:30][CH2:31]2)[N:21]=1

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 11774121HCID 11774121, Verbindung

Produkt 1

HCID 11784673(2-Chloro-9-cyclopentyl-purin-6-yl)-{2-[3-(4-methyl-piperazin-1-yl)-propoxy]-phenyl}-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

[2-(3-Chloro-propoxy)-phenyl]-(2-chloro-9-cyclopentyl-purin-6-yl)-amine (0.4 mmol) are stirred at RT in N-methylpiperazine (0.3 ml) for 12 hours. The mixture is diluted with water and extracted 3 times with ethyl acetate. The combined organic phases are washed with brine and the extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=9:1) as mobile phase. The product containing fractions are combined and evaporated. A pale oil with Rf=0.25 (CH2Cl2/MeOH=9:2) is obtained.

Aufarbeitung

  1. extractionextracted 3 times with ethyl acetate
  2. washThe combined organic phases are washed with brine
  3. dry with materialthe extract is dried over sodium sulfate
  4. customevaporated
  5. customThe residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=9:1) as mobile phase
  6. additionThe product containing fractions
  7. customevaporated
  8. customA pale oil with Rf=0.25 (CH2Cl2/MeOH=9:2) is obtained

Quellen und Nachweise

ORD-Eintrag
ord-38b3b222295e4edebf11192fcf6fabe1
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07544688B2

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