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Potassium Iodide → HCID 44479892, Verbindung

HRID 1647810
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1647810
[CH3:1][S:2]([NH:5][CH2:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[NH:12][CH:11]=[C:10]2[CH2:16][CH2:17][CH2:18]CS([O-])(=O)=O)(=[O:4])=[O:3].[I-].[K+].C(N(CC)C(C)C)(C)C.[CH3:35][O:36][C:37]1[C:38]([N:43]2[CH2:48][CH2:47][NH:46][CH2:45][CH2:44]2)=[N:39][CH:40]=[N:41][CH:42]=1>C(#N)C.C(Cl)Cl>[CH3:35][O:36][C:37]1[C:38]([N:43]2[CH2:48][CH2:47][N:46]([CH2:18][CH2:17][CH2:16][C:10]3[C:9]4[C:13](=[CH:14][CH:15]=[C:7]([CH2:6][NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[CH:8]=4)[NH:12][CH:11]=3)[CH2:45][CH2:44]2)=[N:39][CH:40]=[N:41][CH:42]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 104201525-Methoxy-4-(piperazin-1-yl)pyrimidineHCID 199216343-[5-[[(methylsulfonyl)amino]methyl]-1H-indol-3-yl]propylmethanesulfonate

Produkt 1

HCID 44479892HCID 44479892, VerbindungAusbeute 57 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittel
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of crude 3-[5-[[(methylsulfonyl)amino]methyl]-1H-indol-3-yl]propylmethanesulfonate (15.1 mmol, 1.0 equiv.) in 200 mL of anhydrous acetonitrile were added 2.51 g (15.1 mmol, 1.0 equiv.) of potassium iodide, 3.15 mL of N,N-diisopropylethylamine and 3.23 g of 1-(5-methoxy-4-pyrimidinyl)piperazine. The mixture was heated to reflux for 48 hours. The reaction mixture was cooled to room temperature, filtered and concentrated. The residue was dissolved in 250 mL of chloroform, washed with 50 mL portions of 10% aqueous potassium carbonate and saturated aqueous sodium chloride. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to yield an oil. Chromatography on silica gel using 7.5% methanol in methylene chloride containing 0.75% concentrated aqueous ammonium hydroxide gave 3.93 g (57%) of 4-(5-methoxy-4-pyrimidinyl)-1-[[5-[[(methylsulfonyl)amino]methyl]-1H-indol-3-yl]propyl]piperazine. The hydrochloride was prepared by addition of 3N ethanolic HCl to an ethanolic solution of the base. Recrystallization from ethanol followed by drying in vacuo at 65° C. gave 0.268 g (53%) of the hydrochloride ethanolate: C22H30N6O3S/2.4 HCl/0.4 C2H6O, m.p. 204°-206° C. Elemental analysis calculated C, 48.51; H, 6.21; N, 14.89; found: C, 48.59; H, 6.21; N, 14.95.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 48 hours
  3. filtrationfiltered
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in 250 mL of chloroform
  6. washwashed with 50 mL portions of 10% aqueous potassium carbonate and saturated aqueous sodium chloride
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customto yield an oil

Quellen und Nachweise

ORD-Eintrag
ord-0c4b53a6d64e4f4d808cd2dded4821d0
Quelldatensatz
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05434154

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