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Azepane → 6-Amino-2-(butylamino)-9-[4-(hexahydro-1H-azepin-1-yl)pentyl]-7,9-dihydro-8H-purin-8-one

HRID 590496
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 590496
FC(F)(F)C(O)=O.C(NC1NC2C(N=C(OC)N=2)=C(N)N=1)CCC.C(=O)([O-])[O-].[K+].[K+].BrCCCCCCl.[NH:38]1[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1.C(N(CC)CC)C.[CH2:52]([NH:56][C:57]1[N:65]=[C:64]2[C:60]([N:61]=[C:62]([O:78]C)[N:63]2[CH2:66][CH2:67][CH2:68][CH2:69][CH2:70]N2CCCCCC2)=[C:59]([NH2:80])[N:58]=1)[CH2:53][CH2:54][CH3:55]>CN(C=O)C>[NH2:80][C:59]1[N:58]=[C:57]([NH:56][CH2:52][CH2:53][CH2:54][CH3:55])[N:65]=[C:64]2[C:60]=1[NH:61][C:62](=[O:78])[N:63]2[CH2:66][CH2:67][CH2:68][CH:69]([N:38]1[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1)[CH3:70]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 8119AzepaneHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 960701-Bromo-5-chloropentaneHCID 66726833n2-Butyl-9-[5-(hexahydro-1h-azepin-1-yl)pentyl]-8-(methyloxy)-9h-purine-2,6-diamineHCID 178448877HCID 178448877, Verbindung

Produkt 1

HCID 1176900616-Amino-2-(butylamino)-9-[4-(hexahydro-1H-azepin-1-yl)pentyl]-7,9-dihydro-8H-purin-8-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

N2-Butyl-8-(methyloxy)-3H-purine-2,6-diamine trifluoroacetate (192 mg, 0.547 mmol) and potassium carbonate (189 mg, 1.368 mmol) were suspended in DMF (3 ml) and heated to 60° C. for 1 hour. The reaction mixture was cooled to room temperature and 1-bromo-5-chloropentane (0.072 ml, 0.547 mmol) was added and the reaction stirred for a further 18 hours. Hexahydro-1H-azepine (54.2 mg, 0.547 mmol) and triethylamine (0.076 ml, 0.547 mmol) were added and the reaction mixture heated to 70° C. for 24 hours. LCMS showed a major peak with MH+ 404 consistent with the formation of N2-butyl-9-[5-(hexahydro-1H-azepin-1-yl)pentyl]-8-(methyloxy)-9H-purine-2,6-diamine. The solvent was removed in vacuo and the residue partitioned between DCM (2 ml) and water (2 ml). The aqueous was extracted again with DCM (2 ml) and the combined organic extracts were concentrated and the residue was dissolved in 1:1 MeOH:DMSO (2 ml) and purified by MDAP (Method C). Evaporation of the product containing fractions gave a residual TFA salt which LCMS indicated had undergone hydrolysis of the 8-methoxy group, presumably on concentration in the presence of TFA. This crude material was dissolved once more in 1:1 MeOH:DMSO (2 ml) and re-purified by MDAP (Method A). Product-containing fractions were evaporated under a stream of nitrogen to give the title compound as a white solid (39 mg).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. temperaturethe reaction mixture heated to 70° C. for 24 hours
  3. customThe solvent was removed in vacuo
  4. customthe residue partitioned between DCM (2 ml) and water (2 ml)
  5. extractionThe aqueous was extracted again with DCM (2 ml)
  6. concentrationthe combined organic extracts were concentrated
  7. dissolutionthe residue was dissolved in 1:1 MeOH
  8. customDMSO (2 ml) and purified by MDAP (Method C)
  9. customEvaporation of the product
  10. additioncontaining fractions

Quellen und Nachweise

ORD-Eintrag
ord-1b6c73334d874c1a811079d0c2121884
Quelldatensatz
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09233962B2

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