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Diisopropylamine → 5-(3-Hydroxypropylsulfanyl)-3-methyl-1-(2-methylpropyl)-6-(naphthalen-1-ylmethyl)thieno[2,3-d]pyrimidine-2,4-dione

HRID 1611013
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1611013
C([Li])CCC.C(NC(C)C)(C)C.[CH3:13][N:14]1[C:19](=[O:20])[C:18]2[CH:21]=[C:22]([CH2:24][C:25]3[C:34]4[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=4)[CH:28]=[CH:27][CH:26]=3)[S:23][C:17]=2[N:16]([CH2:35][CH:36]([CH3:38])[CH3:37])[C:15]1=[O:39].CC1C=C[C:44]([S:47](OCCCO[Si](C)(C)C(C)(C)C)(=O)=S)=[CH:43][CH:42]=1.[OH2:62].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1.O>[OH:62][CH2:42][CH2:43][CH2:44][S:47][C:21]1[C:18]2[C:19](=[O:20])[N:14]([CH3:13])[C:15](=[O:39])[N:16]([CH2:35][CH:36]([CH3:37])[CH3:38])[C:17]=2[S:23][C:22]=1[CH2:24][C:25]1[C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH:28]=[CH:27][CH:26]=1
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Komponenten

8

Edukt 5

HCID 7912DiisopropylamineHCID 5282538HCID 5282538, VerbindungHCID 162116731-Butanaminium, N,N,N-tributyl-, fluoride, hydrateHCID 53747051HCID 53747051, VerbindungHCID 178418339Butyllithium

Produkt 1

HCID 5282539
5-(3-Hydroxypropylsulfanyl)-3-methyl-1-(2-methylpropyl)-6-(naphthalen-1-ylmethyl)thieno[2,3-d]pyrimidine-2,4-dione
Ausbeute 39,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel4×

Versuchsvorschrift

Prepared according to the procedure described in Example 5 from n-butyllithium (2.0M solution in hexanes, 0.32 ml) and diisopropylamine (0.093 ml) in anhydrous tetrahydrofuran (5 ml), 3-methyl-1-(2-methylpropyl)-6-(1-naphthalenylmethyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (0.20 g) in anhydrous tetrahydrofuran (5 ml) and 3-{[dimethyl(1,1-dimethylethyl)silyl]oxy}propyl 4-methylphenylthiosulfonate (0.19 g, J. Med. Chem. 1995, 38, 2557) in anhydrous tetrahydrofuran (2 ml). The crude adduct was dissolved in tetrahydrofuran (6 ml) and treated with tetrabutylammonium fluoride hydrate (0.20 g). After 16 hours, the solution was diluted with water (30 ml) and extracted with ether (2×30 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography over silica, eluting with ether and was then recrystallised from ethyl acetate/hexane to give the title compound (0.098 g).

Aufarbeitung

  1. customPrepared
  2. extractionextracted with ether (2×30 ml)
  3. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography over silica
  7. washeluting with ether
  8. customwas then recrystallised from ethyl acetate/hexane

Quellen und Nachweise

ORD-Eintrag
ord-2648734d6e964c4b9748381199f77a93
Quelldatensatz
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06984644B2

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