Sodium Hydroxide → HCID 14257567, Verbindung

HRID 2291952Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2291952
[CH2:1]([N:5]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[S:6]([C:9]1[C:10]2[CH:11]=[CH:12][N:13]=[CH:14][C:15]=2[CH:16]=[CH:17][CH:18]=1)(=[O:8])=[O:7])[C:2]([CH3:4])=O.C([O-])(=O)C.[NH4+].C([BH3-])#[N:31].[Na+].[OH-].[Na+]>C(Cl)(Cl)Cl.CO>[NH2:31][CH:2]([CH3:4])[CH2:1][N:5]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[S:6]([C:9]1[C:10]2[CH:11]=[CH:12][N:13]=[CH:14][C:15]=2[CH:16]=[CH:17][CH:18]=1)(=[O:8])=[O:7]

Komponenten

7

Edukt 4

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 14257566HCID 14257566, Verbindung

Produkt 1

HCID 14257567HCID 14257567, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To 75 ml of an anhydrous methanol solution containing 5.89 g of the thus obtained N-acetonyl-N-hexyl-5-isoquinolinesulfonamide were added 13.03 g of ammonium acetate and 0.75 g of sodium cyanoborohydride, followed by stirring at 15° to 20° C. for 19 hours. Then, the methanol was removed at 30° C. under reduced pressure. To the resultant reaction product were added 50 ml of chloroform and 50 ml of 1N sodium hydroxide solution. The chloroform layer was dried with anhydrous magnesium sulfate, and the chloroform was removed under reduced pressure to obtain a residue. The residue thus obtained was subjected to purification by silica gel column chromatography (Wacogel C-200, 100 g; solvent: chloroform) to obtain 2.75 g of N-(2-aminopropyl)-N-hexyl-5-isoquinolinesulfonamide [Compound (11)]. Compound (11) was analyzed to give the following data.

Aufarbeitung

  1. customThen, the methanol was removed at 30° C. under reduced pressure
  2. customTo the resultant reaction product
  3. dry with materialThe chloroform layer was dried with anhydrous magnesium sulfate
  4. customthe chloroform was removed under reduced pressure
  5. customto obtain a residue
  6. customThe residue thus obtained
  7. customwas subjected to purification by silica gel column chromatography (Wacogel C-200, 100 g; solvent: chloroform)

Quellen und Nachweise

ORD-Eintrag
ord-967116a071bc4e9d92a4bef28f294382
Quelldatensatz
uspto-grants-1989_01
Patentnummer
US04798897

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