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Dichloromethane → HCID 117993077, Verbindung

HRID 922585
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 922585
Br[C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][N:8]2[CH3:11])=[C:4]([Cl:12])[CH:3]=1.CC1(C)COB(B2OCC(C)(C)CO2)OC1.CC([O-])=O.[K+].ClCCl.Cl[C:38]1[N:43]=[C:42]([O:44][CH3:45])[C:41]([C@@:46]2([CH3:53])[CH2:51][CH2:50][CH2:49][NH:48][C:47]2=[O:52])=[CH:40][CH:39]=1.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1>[Cl:12][C:4]1[CH:3]=[C:2]([C:38]2[N:43]=[C:42]([O:44][CH3:45])[C:41]([C@@:46]3([CH3:53])[CH2:51][CH2:50][CH2:49][NH:48][C:47]3=[O:52])=[CH:40][CH:39]=2)[CH:10]=[C:9]2[C:5]=1[CH:6]=[N:7][N:8]2[CH3:11]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 6344Dichloromethane2×HCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2734316Bis(neopentyl glycolato)diboronHCID 117993037HCID 117993037, VerbindungHCID 117993132HCID 117993132, Verbindung

Produkt 1

HCID 117993077
HCID 117993077, Verbindung
Ausbeute 79 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

An oven dried vial was charged with 6-bromo-4-chloro-1-methyl-1H-indazole (507 mg, 2.1 mmol), 5,5,5′,5′-tetramethyl-2,2′-bi(1,3,2-dioxaborinane) (649 mg, 1.9 mmol), oven dried KOAc (604 mg, 6.2 mmol), [1,1′-Bis(diphenylphosphino)-ferrocene]dichloropalladium(II) complex with dichloromethane (54 mg, 0.066 mmol) and dioxane (10 mL), and purged with nitrogen for 20 min. The reaction was heated at 100° C. for 1 h. The mixture was filtered through a pad of Celite®, and the filter cake was rinsed with dioxane. The filtrate was concentrated under reduced pressure to afford the crude residue (530 mg). To a solution of this crude residue (370 mg) in degassed dioxane (2 mL) was added (R)-3-(6-chloro-2-methoxypyridin-3-yl)-3-methylpiperidin-2-one (300 mg, 1.2 mmol), an aqueous solution of sodium carbonate (2 M, 1.5 mL, 2.9 mmol) and [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with dichloromethane (54 mg, 0.066 mmol). The reaction mixture was degassed with nitrogen, and heated at 100° C. for 1 h. The reaction mixture was cooled to r.t., and anhydrous Na2SO4 was added. The mixture was filtered through a pad of Celite®, and the filter cake was rinsed with dioxane. The filtrate was concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (0-100% EtOAc in Heptane to 0-30% EtOH/DCM) to afford (R)-3-(6-(4-chloro-1-methyl-1H-indazol-6-yl)-2-methoxypyridin-3-yl)-3-methylpiperidin-2-one (358 mg, 79%). 1H NMR (600 MHz, CDCl3) δ 1.68 (d, 1H), 1.74 (s, 3H), 1.88 (d, 1H), 1.97-2.07 (m, 1H), 2.39 (td, 1H), 3.37-3.47 (m, 1H), 3.50-3.60 (m, 1H), 4.12 (s, 3H), 4.15 (s, 3H), 5.81 (brs, 1H), 7.42 (d, 1H), 7.70 (d, 1H), 7.82 (s, 1H), 7.94 (s, 1H), 8.06 (s, 1H). MS (AP+)(M+H) 385.

Aufarbeitung

  1. customAn oven dried vial
  2. custompurged with nitrogen for 20 min
  3. filtrationThe mixture was filtered through a pad of Celite®
  4. washthe filter cake was rinsed with dioxane
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customto afford the crude residue (530 mg)
  7. customThe reaction mixture was degassed with nitrogen
  8. temperatureheated at 100° C. for 1 h
  9. temperatureThe reaction mixture was cooled to r.t.
  10. additionanhydrous Na2SO4 was added
  11. filtrationThe mixture was filtered through a pad of Celite®
  12. washthe filter cake was rinsed with dioxane
  13. concentrationThe filtrate was concentrated under reduced pressure
  14. customThe crude product was purified by silica gel column chromatography (0-100% EtOAc in Heptane to 0-30% EtOH/DCM)

Quellen und Nachweise

ORD-Eintrag
ord-d2a0dc0537644e78b41de49ec2c1075e
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09278953B2

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