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Cesium carbonate → HCID 136377184, Verbindung

HRID 1027304
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1027304
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([N:14]3[CH2:18][C@@H:17]4[CH2:19][N:20](C(OC(C)(C)C)=O)[CH2:21][C@@H:16]4[CH2:15]3)=[CH:10][CH:9]=2)=[C:4]([OH:29])[CH:3]=1.CC1(C)C(C)(C)OB([C:38]2[CH:39]=[N:40][N:41](C(OC(C)(C)C)=O)[CH:42]=2)O1.C([O-])([O-])=O.[Cs+].[Cs+].O1CCOCC1>CC(C1C=C(C(C)C)C(C2C(OC)=CC(Cl)=C(OC)C=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.[Pd+2].O>[CH2:15]1[C@@H:16]2[CH2:21][NH:20][CH2:19][C@@H:17]2[CH2:18][N:14]1[C:11]1[N:12]=[N:13][C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:38]3[CH:39]=[N:40][NH:41][CH:42]=3)=[CH:3][C:4]=2[OH:29])=[CH:9][CH:10]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 10796Cesium carbonateHCID 312751,4-DioxaneHCID 16217654tert-butyl 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylateHCID 136377183HCID 136377183, Verbindung

Produkt 1

HCID 136377184HCID 136377184, VerbindungAusbeute 51,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 75412134Dicyclohexyl(2 inverted exclamation mark,4 inverted exclamation mark,6 inverted exclamation mark-Triisopropyl-3,6-Dimethoxy-[1,1 inverted exclamation mark-Biphenyl]-2-Yl)Phosphine-(2-(2-Aminoethyl)Phenyl)Palladium(Ii) ChlorideKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

To a 10 mL microwave vial, was added (3aR,6aS)-tert-butyl 5-(6-(4-chloro-2-hydroxyphenyl)pyridazin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (0.182 g, 0.437 mmol), tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylate (0.385 g, 1.310 mmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′,4′,6′-triisopropyl-1,1′-biphenyl][2-(2-aminoethyl)phenyl]palladium(II) (0.035 g, 0.044 mmol) and Cs2CO3 (0.427 g, 1.310 mmol), followed by adding 1,4-dioxane (2 mL) and water (0.5 mL). The reaction mixture was evacuated and filled with N2 twice then heated at 90° C. overnight. The reaction mixture was filtered through celite and washed with DMSO and MeOH. The filtrate was acidified with 1N HCl and stirred at RT for 3 hour, then extracted with DCM. The aqueous layer was basified with 2M NH2 in MeOH and a brownish precipitate formed, which was filtered and washed with DMSO to afford a grey solid 2-(6-((3aR,6aS)-hexahydropyrrolo[3,4-c]pyrrol-2(1H)-yl)pyridazin-3-yl)-5-(1H-pyrazol-4-yl)phenol (82 mg, 0.224 mmol, 51.2% yield). MS (M+1)=349.1. The DMSO wash solution was concentrated to afford a DMSO solution of desired (3aR,6aS)-tert-butyl 5-(6-(2-hydroxy-4-(1H-pyrazol-4-yl)phenyl)pyridazin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (75 mg, 0.167 mmol, 38% yield), MS (M+1)=449.1, which was used directly in the next step.

Aufarbeitung

  1. customThe reaction mixture was evacuated
  2. additionfilled with N2 twice
  3. filtrationThe reaction mixture was filtered through celite
  4. washwashed with DMSO and MeOH
  5. extractionextracted with DCM
  6. customa brownish precipitate formed
  7. filtrationwhich was filtered
  8. washwashed with DMSO

Quellen und Nachweise

ORD-Eintrag
ord-9acbf1474aaa4c33b9c0c05ea553976e
Quelldatensatz
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08729263B2

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