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Potassium Phosphate, Tribasic → HCID 57454141, Verbindung

HRID 546948
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 546948
C([Si](C)(C)[O:6][C:7]([C:42]([F:45])([F:44])[F:43])([C:38]([F:41])([F:40])[F:39])/[CH:8]=[CH:9]/[C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:21]2[CH:26]=[CH:25][C:24](B3OC(C)(C)C(C)(C)O3)=[C:23]([CH3:36])[CH:22]=2)([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:12][C:11]=1[CH3:37])(C)(C)C.[CH2:48]([O:50][C:51](=[O:60])[CH2:52][C:53]1[CH:54]=[N:55][C:56](Br)=[N:57][CH:58]=1)[CH3:49].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>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.O>[CH2:48]([O:50][C:51](=[O:60])[CH2:52][C:53]1[CH:54]=[N:55][C:56]([C:24]2[CH:25]=[CH:26][C:21]([C:16]([CH2:19][CH3:20])([C:13]3[CH:14]=[CH:15][C:10](/[CH:9]=[CH:8]/[C:7]([OH:6])([C:42]([F:44])([F:45])[F:43])[C:38]([F:41])([F:40])[F:39])=[C:11]([CH3:37])[CH:12]=3)[CH2:17][CH3:18])=[CH:22][C:23]=2[CH3:36])=[N:57][CH:58]=1)[CH3:49]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 62657Potassium Phosphate, TribasicHCID 57443494Ethyl 2-(2-bromopyrimidin-5-yl)acetateHCID 57709023HCID 57709023, Verbindung

Produkt 1

HCID 57454141HCID 57454141, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397
HCID 178418397, Verbindung
Katalysator
HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
95.5 °C

Versuchsvorschrift

Degassed N,N-dimethylformamide (0.32 mL) was added to 2-[4-(1-{4-[(E)-3-(t-butyl-dimethyl-silanyloxy)-4,4,4-trifluoro-3-trifluoromethyl-1-butenyl]-3-methyl-phenyl}-1-ethyl-propyl)-2-methyl-phenyl]-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (Example 77-(1); 35.8 mg, 0.0523 mmol), 2-bromopyrimidine-5-acetic acid ethyl ester (Example 43-(3); 37.3 mg, 0.152 mmol), tetrakis(triphenylphosphine)palladium (0) (29.8 mg, 0.0258 mmol) and potassium phosphate (48.7 mg, 0.229 mmol). After replacement with nitrogen, the mixture was heated while stirring at an external temperature of 91 to 100° C. for 10 hours. Water was added to the reaction mixture, followed by extraction with diethyl ether. The extract was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=4/1) to give the title compound (13 mg, 41%).

Aufarbeitung

  1. customDegassed N,N-dimethylformamide (0.32 mL)
  2. temperatureAfter replacement with nitrogen, the mixture was heated
  3. extractionfollowed by extraction with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate=4/1)

Quellen und Nachweise

ORD-Eintrag
ord-610b11214dc440febaf0223b2a15078a
Quelldatensatz
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07935688B2

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