Triethylamine → HCID 20159875, Verbindung

HRID 247576Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 247576
[NH2:1][CH2:2][CH:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:4][NH2:5].C(N(CC)CC)C.[CH:19]1[C:28]2[CH:27]=[CH:26][CH:25]=[C:24]([S:29](Cl)(=[O:31])=[O:30])[C:23]=2[CH:22]=[CH:21][N:20]=1.CO.C(Cl)(Cl)Cl>C(Cl)(Cl)Cl>[NH2:1][CH2:2][CH:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:4][NH:5][S:29]([C:24]1[C:23]2[CH:22]=[CH:21][N:20]=[CH:19][C:28]=2[CH:27]=[CH:26][CH:25]=1)(=[O:30])=[O:31]

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 5687002-Phenyl-1,3-propanediamineHCID 33716555-Isoquinolinesulfonyl chlorideHCID 21584188Chloroform methanol

Produkt 1

HCID 20159875HCID 20159875, VerbindungAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel3×

Versuchsvorschrift

In 50 ml of a chloroform solution containing 11.55 g of 1,3-diamino-2-phenylpropane and 1.33 g of triethylamine was added dropwise 30 ml of a chloroform solution containing 3.5 g of 5-isoquinolinesulfonyl chloride under cooling with ice. After the dropwise addition of the chloroform solution, the mixed solution was stirred at a temperature of 10° C. to 20° C. for four hours, and the reaction mixture solution was washed with water and dried with anhydrous potassium carbonate. After the chloroform was distilled therefrom, the residue thus obtained was subjected to a silica gel column chromatography (silica gel: 90 g; solvent: 5% methanol/chloroform (volume ratio)) to give 3.20 g of N-(3-amino-2-phenylpropyl)-5-isoquinolinesulfonamide in a yield of 61%.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. washthe reaction mixture solution was washed with water
  3. dry with materialdried with anhydrous potassium carbonate
  4. distillationAfter the chloroform was distilled
  5. customthe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-79f0e0d9be5145f69418194f0eab7fdd
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04709032

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