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Binap, (A+-)- → 1,1,1-Trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-[({6-methyl-1-[4-(methyloxy)phenyl]-1H-indazol-4-yl}amino)methyl]-2-pentanol

HRID 418804
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 418804
[NH2:1][CH2:2][C:3]([OH:21])([CH2:8][C:9]([C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:13]=1[O:19][CH3:20])([CH3:11])[CH3:10])[C:4]([F:7])([F:6])[F:5].Br[C:23]1[CH:31]=[C:30]([CH3:32])[CH:29]=[C:28]2[C:24]=1[CH:25]=[N:26][N:27]2[C:33]1[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[CH:35][CH:34]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[F:5][C:4]([F:7])([F:6])[C:3]([CH2:2][NH:1][C:23]1[CH:31]=[C:30]([CH3:32])[CH:29]=[C:28]2[C:24]=1[CH:25]=[N:26][N:27]2[C:33]1[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[CH:35][CH:34]=1)([OH:21])[CH2:8][C:9]([C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:13]=1[O:19][CH3:20])([CH3:11])[CH3:10]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 634876Binap, (A+-)-HCID 179365862-(Aminomethyl)-1,1,1-trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-pentanol2×HCID 23676156Sodium t-butoxideHCID 576159621h-Indazole,4-bromo-1-(4-methoxyphenyl)-6-methyl-2×

Produkt 1

HCID 57615926
1,1,1-Trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-[({6-methyl-1-[4-(methyloxy)phenyl]-1H-indazol-4-yl}amino)methyl]-2-pentanol
Ausbeute 59,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a mixture of 2-(aminomethyl)-1,1,1-trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-pentanol (Intermediate 18, 200 mg, 0.65 mmol) and 4-bromo-6-methyl-1-[4-(methyloxy)phenyl]-1H-indazole (Intermediate 15, 190 mg, 0.6 mmol) in toluene (3 mL) were added tris(dibenzylideneacetone)dipalladium(0) (28 mg, 0.03 mmol), racemic-BINAP (37 mg, 0.06 mmol) and sodium tert-butoxide (85 mg, 0.84 mmol). The mixture was heated in a microwave at 120° C. for 30 min and then cooled and partitioned between ethyl acetate (60 mL) and 1M hydrochloric acid (60 mL). The organic layer was separated, washed sequentially with aqueous sodium bicarbonate (30 mL) and brine (30 mL), passed through a hydrophobic frit and evaporated under reduced pressure. The residue was dissolved in dichloromethane (1.5 mL) and loaded onto a silica SPE cartridge and eluted with a gradient of ethyl acetate:petroleum ether (1:9 to 1:4) to give the title compound (194 mg).

Aufarbeitung

  1. temperaturecooled
  2. custompartitioned between ethyl acetate (60 mL) and 1M hydrochloric acid (60 mL)
  3. customThe organic layer was separated
  4. washwashed sequentially with aqueous sodium bicarbonate (30 mL) and brine (30 mL)
  5. customevaporated under reduced pressure
  6. dissolutionThe residue was dissolved in dichloromethane (1.5 mL)
  7. washeluted with a gradient of ethyl acetate:petroleum ether (1:9 to 1:4)

Quellen und Nachweise

ORD-Eintrag
ord-3f9a0139820b429d8fdf4fcb6f5044c6
Quelldatensatz
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08093281B2

Notizen zur Reaktion

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