Hydrochloric Acid → 6-Amino-2-(butylamino)-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-7,9-dihydro-8H-purin-8-one

HRID 1011173Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1011173
[CH2:1]([NH:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:24]C)[N:12]2[CH2:15][CH:16]2[CH2:21][CH2:20][O:19][C:18]([CH3:23])([CH3:22])[CH2:17]2)=[C:8]([NH2:26])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl>CO.O1CCOCC1>[NH2:26][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:24])[N:12]2[CH2:15][CH:16]1[CH2:21][CH2:20][O:19][C:18]([CH3:23])([CH3:22])[CH2:17]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 57699692N2-Butyl-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-8-methoxy-9H-purine-2,6-diamine

Produkt 1

HCID 576997186-Amino-2-(butylamino)-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-7,9-dihydro-8H-purin-8-oneAusbeute 52,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of N2-butyl-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-8-methoxy-9H-purine-2,6-diamine (73 mg) in MeOH (2 mL) was treated with 4N HCl in 1,4-dioxane (1 mL) and was stirred for 4 h. The reaction was evaporated and the residue treated with water then basified with saturated sodium bicarbonate solution. The resulting solid was filtered, washed with water and dried. The solid was re-precipitated from ether/light petrol to give the title compound (37 mg).

Aufarbeitung

  1. customThe reaction was evaporated
  2. additionthe residue treated with water
  3. filtrationThe resulting solid was filtered
  4. washwashed with water
  5. customdried
  6. customThe solid was re-precipitated from ether/light petrol

Quellen und Nachweise

ORD-Eintrag
ord-d6f777a6bab7490680745212478bb275
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977344B2

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