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Dicyclohexylamine → N-benzyl-2-chloro-7-ethynylthieno[3,2-d]pyrimidin-4-amine

HRID 1485503
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1485503
[CH2:1]([NH:8][C:9]1[C:10]2[S:18][CH:17]=[C:16](Br)[C:11]=2[N:12]=[C:13]([Cl:15])[N:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:20]1(NC2CCCCC2)CCCC[CH2:21]1.C([Si](C)(C)C)#C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1>C(#N)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I>[CH2:1]([NH:8][C:9]1[C:10]2[S:18][CH:17]=[C:16]([C:20]#[CH:21])[C:11]=2[N:12]=[C:13]([Cl:15])[N:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 7582DicyclohexylamineHCID 8028TetrahydrofuranHCID 66111TrimethylsilylacetyleneHCID 2724141Tetrabutylammonium FluorideHCID 86675658N-benzyl-7-bromo-2-chlorothieno[3,2-d]pyrimidin-4-amine

Produkt 1

HCID 86675659N-benzyl-2-chloro-7-ethynylthieno[3,2-d]pyrimidin-4-amine
Ausbeute 68,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 178418476HCID 178418476, VerbindungKatalysatorHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

N-Benzyl-7-bromo-2-chlorothieno[3,2-d]pyrimidin-4-amine (310 mg, 0.874 mmol) was dissolved in acetonitrile (4 mL) and then bis(triphenylphosphine)palladium(II) dichloride (15 mg, 0.022 mmol), CuI (6 mg, 0.350 mmol), dicyclohexylamine (0.19 mL, 0.96 mmol) and ethynyltrimethylsilane (0.24 mL, 1.75 mmol) were added. After flowing nitrogen gas for 15 minutes, the reaction mixture was stirred at 80° C. for 14 hours. After cooling to room temperature, the reaction mixture was filtered with celite and washed with ethyl acetate (50 mL). The filtrate was washed with brine and concentrated by drying with MgSO4. Without purification, the resultant compound was dissolved in anhydrous tetrahydrofuran (5 mL) and then 1.0 M tetrabutylammonium fluoride dissolved in tetrahydrofuran (4.4 mL, 4.4 mmol) was added thereto. The reaction mixture was stirred at room temperature for 30 minutes and then concentrated. Purification of the mixture by silica gel chromatography (ethyl acetate/hexane: 2/8→3/7) yielded the target compound (180 mg, 68% yield).

Aufarbeitung

  1. customfor 15 minutes
  2. temperatureAfter cooling to room temperature
  3. filtrationthe reaction mixture was filtered with celite
  4. washwashed with ethyl acetate (50 mL)
  5. washThe filtrate was washed with brine
  6. concentrationconcentrated
  7. dry with materialby drying with MgSO4
  8. customWithout purification
  9. dissolutionthe resultant compound was dissolved in anhydrous tetrahydrofuran (5 mL)
  10. additionwas added
  11. stirringThe reaction mixture was stirred at room temperature for 30 minutes
  12. concentrationconcentrated
  13. customPurification of the mixture by silica gel chromatography (ethyl acetate/hexane: 2/8→3/7)

Quellen und Nachweise

ORD-Eintrag
ord-2f47bbf94bb74b86bcec03cfd95b4494
Quelldatensatz
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09422307B2

Notizen zur Reaktion

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