Hydrochloric Acid → 6-Amino-2-butylamino-9-(tetrahydro-2H-Pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011150

Reaktionsgleichung

Reaktionsgleichung von HRID 1011150
[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][O:19][CH2:18][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[CH2:17][CH2:18][O:19][CH2:20][CH2:21]1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57699729N2-Butyl-8-methoxy-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-Purine-2,6-diamine

Produkt 1

HCID 248845276-Amino-2-butylamino-9-(tetrahydro-2H-Pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-oneAusbeute 57,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of N2-butyl-8-methoxy-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine-2,6-diamine (310 mg) in dry methanol (30 ml) at room temperature and under nitrogen was added 4.0M hydrogen chloride in 1,4-dioxane (5.5 ml) in one go. The reaction was left to stir at room temperature for 16 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 (10 ml) and the solid filtered and dried on the rotary evaporator (60° C.) for 30 minutes. This afforded the title compound as a solid (170 mg).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-607006ab63754d7796a344b7aac7b5ba
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977344B2

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