Water → HCID 178513008, Verbindung

HRID 247584

Reaktionsgleichung

Reaktionsgleichung von HRID 247584
[NH2:1][CH2:2][CH2:3][NH:4][S:5]([C:8]1[C:9]2[CH:10]=[CH:11][N:12]=[CH:13][C:14]=2[CH:15]=[CH:16][CH:17]=1)(=[O:7])=[O:6].O.S(O)(O)(=O)=O.CS[C:26](=[NH:28])[NH2:27].[OH-].[Na+]>CO>[NH:1]([CH2:2][CH2:3][NH:4][S:5]([C:8]1[C:9]2[CH:10]=[CH:11][N:12]=[CH:13][C:14]=2[CH:15]=[CH:16][CH:17]=1)(=[O:7])=[O:6])[C:26]([NH2:28])=[NH:27]

Komponenten

6

Edukt 4

HCID 962WaterHCID 3544N-(2-Aminoethyl)isoquinoline-5-sulfonamideHCID 14798Sodium HydroxideHCID 752702-Methyl-2-thiopseudourea sulfate

Produkt 1

HCID 178513008HCID 178513008, VerbindungAusbeute 84,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

In 30 ml of methanol was dissolved 3.3 g of N-(2-aminoethyl)-5-isoquinolinesulfonamide obtained in Referential example 1, and to the solution was added 25 ml of water solution containing 5.0 g of S-methylisothiourea sulfate. And to the mixed solution was added 1N aqueous sodium hydroxide solution, the mixed solution thus obtained was heated at reflux for two hours. After the reflux, the methanol was distilled therefrom under reduced pressure, and the white crystals precipitated were separated by filtration under reduced pressure. The crystalline residue thus obtained was recrystallized from methanol to give 3.24 g of N-(2-guanidinoethyl)-5-isoquinolinesulfonamide, i.e., Compound (2) in a yield of 84%.

Aufarbeitung

  1. customobtained in Referential example 1
  2. customthe mixed solution thus obtained
  3. temperaturewas heated
  4. temperatureat reflux for two hours
  5. distillationAfter the reflux, the methanol was distilled
  6. customunder reduced pressure, and the white crystals precipitated
  7. customwere separated by filtration under reduced pressure
  8. customThe crystalline residue thus obtained
  9. customwas recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-a3d115384dbb41d79a84fc75fcc3c33c
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04709032

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