Chloroform → 1-(5-Isoquinolinesulfonyl)-2,5-dimethylpiperazine

HRID 1248759

Reaktionsgleichung

Reaktionsgleichung von HRID 1248759
[CH3:1][CH:2]1[CH2:7][NH:6][CH:5]([CH3:8])[CH2:4][NH:3]1.C(N(CC)CC)C.[CH:16]1[C:25]2[CH:24]=[CH:23][CH:22]=[C:21]([S:26](Cl)(=[O:28])=[O:27])[C:20]=2[CH:19]=[CH:18][N:17]=1.C(Cl)(Cl)Cl>C(Cl)Cl>[CH:16]1[C:25]2[CH:24]=[CH:23][CH:22]=[C:21]([S:26]([N:3]3[CH2:4][CH:5]([CH3:8])[NH:6][CH2:7][CH:2]3[CH3:1])(=[O:28])=[O:27])[C:20]=2[CH:19]=[CH:18][N:17]=1

Komponenten

6

Edukt 4

HCID 6212ChloroformHCID 78162,5-DimethylpiperazineHCID 8471TriethylamineHCID 33716555-Isoquinolinesulfonyl chloride

Produkt 1

HCID 132291781-(5-Isoquinolinesulfonyl)-2,5-dimethylpiperazineAusbeute 59,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Versuchsvorschrift

In 30 ml of methylene chloride were dissolved 1.75 g of 2,5-dimethylpiperazine and 1.53 g of triethylamine, and to the solution was added dropwise 20 ml of a methylene chloride solution containing 1.73 g of 5-isoquinolinesulfonyl chloride under cooling with ice. After the dropwise addition of the methylene chloride solution, the mixed solution obtained was stirred at a temperature of 5° C. to 10° C. for three hours, and then the reaction mixture solution was washed with water and dried with anhydrous magnesium sulfate. After the methylene chloride was distilled therefrom, the residue obtained was subjected to an alumina column chromatography (alumina: 50 g; solvent: chloroform) to give 1.38 g of 1-(5-isoquinolinesulfonyl)-2,5-dimethylpiperazine, Compound (40) in a yield of 59%.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. customthe mixed solution obtained
  3. washthe reaction mixture solution was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. distillationAfter the methylene chloride was distilled
  6. customthe residue obtained

Quellen und Nachweise

ORD-Eintrag
ord-020d59c94ab748d79eb7930b6789cd81
Quelldatensatz
uspto-grants-1985_06
Patentnummer
US04525589

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