StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Diisopropylamine → (2R)-1-[2-(5-bromo-1-benzofuran-2-yl)ethyl]-2-methylpyrrolidine

HRID 2416137
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2416137
[C:1]([CH:4]([CH:6]([C:8](O)=O)O)O)(O)=O.[CH3:11][C@@H:12]1[CH2:16][CH2:15][CH2:14][NH:13]1.C(=O)([O-])[O-].[K+].[K+].CC1C=CC(S(OCCC#C)(=O)=O)=CC=1.[Br:38][C:39]1[CH:44]=[CH:43][C:42]([OH:45])=[C:41](I)[CH:40]=1.C(NC(C)C)(C)C>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)I>[Br:38][C:39]1[CH:44]=[CH:43][C:42]2[O:45][C:4]([CH2:6][CH2:8][N:13]3[CH2:14][CH2:15][CH2:16][C@H:12]3[CH3:11])=[CH:1][C:41]=2[CH:40]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 7912DiisopropylamineHCID 11430Potassium CarbonateHCID 2720203-Butynyl p-toluenesulfonateHCID 109245324-Bromo-2-iodophenolHCID 23404464(2R)-2-Methylpyrrolidine tartrate

Produkt 1

HCID 11220543(2R)-1-[2-(5-bromo-1-benzofuran-2-yl)ethyl]-2-methylpyrrolidine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 83717Copper iodideKatalysatorHCID 178418476HCID 178418476, VerbindungKatalysatorHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

(2R)-2-Methylpyrrolidine tartrate (1.17 g, 5.0 mmol), and potassium carbonate (1.38 g, 10.0 mmol) were combined in acetonitrile (20 mL) and heated at 60° C. for 1 hour. The mixture was treated with 3-butynyl 4-methylbenzenesulfonate (673 mg, 3.0 mmol) and heated at about 60° C. overnight. The mixture was cooled to about 5° C. and filtered. The mixture was treated with the product from Example 3A (300 mg, 1.0 mmol), diisopropylamine (1.20 g, 11.8 mmol), dichlorobis(triphenylphosphine)palladium (II) (35.1 mg, 0.05 mmol), and copper iodide (38.0 mg, 0.20 mmol). After stirring overnight at about 30° C., the mixture was concentrated to dryness. The residue in ethyl acetate (20 mL) was washed with 5% NaHCO3 (20 mL×2) and 25% brine (25 mL). The organic phase was separated, dried over anhydrous Na2SO4, filtered, and the filtrate concentrated to dryness to provide the title compound. MS (esi): 308, 310 (M+H)+; 1H-NMR (CDCl3) δ 7.58 (1H, d, J=1.7 Hz), 7.27 (2H, m), 6.38 (1H, s), 3.20 (2H, m), 2.95 (2H, m), 2.43 (1H, m), 2.28 (1H, m), 2.19 (1H, q, J=8.8 Hz), 1.95 (1H, m), 1.75 (2H, m), 1.42 (1H, m), 1.13 (3H, d, J=6.2 Hz); 13C-NMR (CDCl3) δ 158.8, 152.9,130.6, 125.7, 122.6, 115.2,111.9, 101.8, 60.0, 53.9, 51.9, 32.9, 28.4, 22.0, 19.3.

Aufarbeitung

  1. temperatureheated at about 60° C. overnight
  2. temperatureThe mixture was cooled to about 5° C.
  3. filtrationfiltered
  4. concentrationthe mixture was concentrated to dryness
  5. washThe residue in ethyl acetate (20 mL) was washed with 5% NaHCO3 (20 mL×2) and 25% brine (25 mL)
  6. customThe organic phase was separated
  7. dry with materialdried over anhydrous Na2SO4
  8. filtrationfiltered
  9. concentrationthe filtrate concentrated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-4719ed18c1af4091abfc23a7f991e5a7
Quelldatensatz
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06822101B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion