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Water → HCID 44555604, Verbindung

HRID 885047
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 885047
Br[C:2]1[N:3]=[CH:4][C:5]([O:31][CH3:32])=[C:6]2[C:10]([C:11](=[O:30])[C:12]([N:14]3[CH2:23][CH2:22][C:21]4[C:16](=[CH:17][CH:18]=[CH:19][C:20]=4[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=4)[CH2:15]3)=[O:13])=[CH:9][NH:8][C:7]=12.[OH2:33].[CH2:34]([N:36]([CH2:39]C)CC)C.CN>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O1CCOCC1>[CH3:32][O:31][C:5]1[CH:4]=[N:3][C:2]([C:34]([NH:36][CH3:39])=[O:33])=[C:7]2[NH:8][CH:9]=[C:10]([C:11](=[O:30])[C:12](=[O:13])[N:14]3[CH2:23][CH2:22][C:21]4[C:16](=[CH:17][CH:18]=[CH:19][C:20]=4[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=4)[CH2:15]3)[C:6]=12
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 6329MethylamineHCID 8471TriethylamineHCID 580260391-(7-bromo-4-methoxy-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-(5-(pyridin-2-yl)-3,4-dihydroisoquinolin-2(1H)-yl)ethane-1,2-dione

Produkt 1

HCID 44555604HCID 44555604, VerbindungAusbeute 32,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397HCID 178418397, VerbindungKatalysator
HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a stainless steel pressure vessel containing 1-(7-bromo-4-methoxy-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-(5-(pyridin-2-yl)-3,4-dihydroisoquinolin-2(1H)-yl)ethane-1,2-dione (0.2 g, 0.407 mmol) was added 1,4-dioxane (5 mL), water (0.037 mL, 2.035 mmol), tetrakis(triphenylphosphine)palladium(0) (0.071 g, 0.061 mmol), triethylamine (0.567 mL, 4.07 mmol), and methylamine (2M in THF) (2.035 mL, 4.07 mmol). The vessel was sealed and purged with N2 3 times. The vessel was filled with carbon monoxide to 50 psi, and purged 2 times, then finally was filled to 80 psi of carbon monoxide. The vessel was heated to 80° C. for 16 h then was cooled to rt. The mixture was transferred to a rb flask and the solvent was removed under reduced pressure. The residue was dissolved in DMF and was passed through a plug of CELITE® to remove the solids. The DMF solution was purified by prep HPLC. The fractions containing the expected product were concentrated under reduced pressure. The residue was dissolved in dichloromethane and was partitioned with aq. sat. NaHCO3. The organic layer was collected, and dried with MgSO4. The drying agent was removed by filtration and the organic solution was concentrated under reduced pressure. The residue was purified by BIOTAGE® flash chromatography using a 0-5% MeOH in dichloromethane gradient using a BIOTAGE® flash chromatography. The expected product, 4-methoxy-N-methyl-3-(2-oxo-2-(5-(pyridin-2-yl)-3,4-dihydroisoquinolin-2(1H)-yl)acetyl)-1H-pyrrolo[2,3-c]pyridine-7-carboxamide (0.065 g, 0.133 mmol, 32.7% yield), was isolated as an off-white solid. LC/MS: m/z 470.24 (M+H)+, 1.582 min (method 1). 1H NMR (500 MHz, DMSO-d6) δ ppm 11.13 (br. s., 1H) 8.60-8.77 (m, 1H) 8.14-8.26 (m, 1H) 7.70-7.94 (m, 3H) 7.02-7.47 (m, 5H) 4.73-5.01 (m, 2H) 3.88-3.97 (m, 3H) 3.66-3.88 (m, 2H) 2.92-3.11 (m, 5H).

Aufarbeitung

  1. customThe vessel was sealed
  2. custompurged with N2 3 times
  3. additionThe vessel was filled with carbon monoxide to 50 psi
  4. custompurged 2 times
  5. additionfinally was filled to 80 psi of carbon monoxide
  6. temperaturethen was cooled to rt
  7. customThe mixture was transferred to a rb flask
  8. customthe solvent was removed under reduced pressure
  9. dissolutionThe residue was dissolved in DMF
  10. customto remove the solids
  11. customThe DMF solution was purified by prep HPLC
  12. additionThe fractions containing the expected product
  13. concentrationwere concentrated under reduced pressure
  14. dissolutionThe residue was dissolved in dichloromethane
  15. customwas partitioned with aq. sat. NaHCO3
  16. customThe organic layer was collected
  17. dry with materialdried with MgSO4
  18. customThe drying agent was removed by filtration
  19. concentrationthe organic solution was concentrated under reduced pressure
  20. customThe residue was purified by BIOTAGE® flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-28d8a6e5d0524db4b30770ab7acec010
Quelldatensatz
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08242124B2

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