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Dichloromethane → 2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-6-(5-methyl-1H-pyrazol-4-yl)-5H-pyrrolo[2,3-b]pyrazine

HRID 1052313
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1052313
Br[C:2]1[N:24](S(C2C=CC=CC=2)(=O)=O)[C:5]2=[N:6][CH:7]=[C:8]([CH2:10][CH2:11][C:12]3[C:17]([F:18])=[C:16]([O:19][CH3:20])[CH:15]=[C:14]([O:21][CH3:22])[C:13]=3[F:23])[N:9]=[C:4]2[CH:3]=1.[CH3:34][C:35]1[C:39](B(O)O)=[CH:38][NH:37][N:36]=1.ClCCl.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C(=O)([O-])[O-].[K+].[K+]>O.Cl[Pd]Cl.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2].O1CCOCC1>[F:18][C:17]1[C:16]([O:19][CH3:20])=[CH:15][C:14]([O:21][CH3:22])=[C:13]([F:23])[C:12]=1[CH2:11][CH2:10][C:8]1[N:9]=[C:4]2[CH:3]=[C:2]([C:39]3[CH:38]=[N:37][NH:36][C:35]=3[CH3:34])[NH:24][C:5]2=[N:6][CH:7]=1
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Komponenten

9

Edukt 5

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 62657Potassium Phosphate, TribasicHCID 899635876-bromo-2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-5-(phenylsulfonyl)-5H-pyrrolo[2,3-b]pyrazineHCID 178434488HCID 178434488, Verbindung

Produkt 1

HCID 73054235
2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-6-(5-methyl-1H-pyrazol-4-yl)-5H-pyrrolo[2,3-b]pyrazine
Ausbeute 46 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)KatalysatorHCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
88 °C

Versuchsvorschrift

A stirred mixture of 6-bromo-2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-5-(phenylsulfonyl)-5H-pyrrolo[2,3-b]pyrazine (15 mg, 28 μmol), (3-methyl-1H-pyrazol-4-yl)boronic acid (4.2 mg, 33 μmol), [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II) complexed with dichloromethane (1:1) (1.8 mg, 2.2 μmol), and potassium phosphate (9.5 mg, 45 mmol) in water (0.2 mL)/1,4-dioxane (1 mL) was heated at 88° C. After 1 hour, the volatiles were removed under vacuum and the residue was dissolved in methanol (1 mL). Potassium carbonate (7.7 mg, 56 μmol) was added and the reaction mixture was warmed up to 60° C. After 0.5 hour, the reaction mixture was cooled to ambient temperature and was purified on RP-HPLC (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.05% TFA, at flow rate of 30 mL/min) to give the desired product (5.1 mg, 46%) as its TFA salt. LCMS calculated for C20H20F2N5O2 (M+H)+: m/z=400.2. Found: 400.2.

Aufarbeitung

  1. customthe volatiles were removed under vacuum
  2. dissolutionthe residue was dissolved in methanol (1 mL)
  3. temperaturethe reaction mixture was warmed up to 60° C
  4. waitAfter 0.5 hour
  5. temperaturethe reaction mixture was cooled to ambient temperature
  6. customwas purified on RP-HPLC (XBridge C18 column
  7. washeluting with a gradient of acetonitrile/water containing 0.05% TFA, at flow rate of 30 mL/min)

Quellen und Nachweise

ORD-Eintrag
ord-5c060d9a9eee4f50a3582977c518e727
Quelldatensatz
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09388185B2

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