Hydrochloric Acid → 6-Amino-2-butylamino-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011154Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1011154
[CH2:1]([NH:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:22]C)[N:12]2[CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][O:18][CH2:17]2)=[C:8]([NH2:24])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.[OH-].[Na+]>CO.O1CCOCC1>[NH2:24][C:8]1[N:7]=[C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:22])[N:12]2[CH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][O:18][CH2:17]1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57699736N2-Butyl-8-methoxy-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purine-2,6-diamine

Produkt 1

HCID 250251666-Amino-2-butylamino-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-oneAusbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of N2-butyl-8-methoxy-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purine-2,6-diamine (45 mg) in dry methanol (3 ml) at room temperature and under nitrogen was added 4.0M hydrogen chloride in 1,4-dioxane (0.7 ml) in one go. The reaction was left to stir at room temperature for 3 hours. The reaction was neutralised by the addition of 2.0M sodium hydroxide solution and concentrated in vacuo. The residue was taken up in water (5 ml) and the solid filtered and dried in vacuo (60° C.) for 30 minutes. This afforded the title compound as a solid (25 mg).

Aufarbeitung

  1. waitThe reaction was left
  2. concentrationconcentrated in vacuo
  3. filtrationthe solid filtered
  4. customdried in vacuo (60° C.) for 30 minutes

Quellen und Nachweise

ORD-Eintrag
ord-31cba9359a184899b047064ebac93e32
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977344B2

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