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Pivalic acid → 4-(5-(4-(Heptyloxy)phenyl)thiazol-2-yl)benzaldehyde

HRID 1775819
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1775819
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[O:11])=[CH:8][CH:7]=1.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1.C(O)(=O)C(C)(C)C.C(=O)([O-])[O-].[K+].[K+].Br[C:47]1[CH:52]=[CH:51][C:50]([O:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH3:60])=[CH:49][CH:48]=1>CC(N(C)C)=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:54]([O:53][C:50]1[CH:49]=[CH:48][C:47]([C:5]2[S:1][C:2]([C:6]3[CH:7]=[CH:8][C:9]([CH:10]=[O:11])=[CH:12][CH:13]=3)=[N:3][CH:4]=2)=[CH:52][CH:51]=1)[CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH3:60]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 6417Pivalic acidHCID 11430Potassium CarbonateHCID 75806TricyclohexylphosphineHCID 5991021-(4-Bromophenoxy)heptaneHCID 105356554-(1,3-Thiazol-2-yl)benzaldehyde

Produkt 1

HCID 866896684-(5-(4-(Heptyloxy)phenyl)thiazol-2-yl)benzaldehyde
Ausbeute 38,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 167845palladium(II) acetateKatalysatorHCID 31374DimethylacetamideLösungsmittel2×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a stirring suspension of 4-(thiazol-2-yl)benzaldehyde (349 mg, 1.84 mmol), tricyclohexylphosphine (27 mg, 0.07 mmol), pivalic acid (64.2 μl, 0.55 mmol), potassium carbonate (382 mg, 2.77 mmol) and palladium (II) acetate (8 mg, 0.04 mmol) in DMA (5.15 mL) under nitrogen was added a solution of 1-bromo-4-(heptyloxy)benzene (500 mg, 1.84 mmol) in DMA (1 mL). The reaction mixture was evacuated and purged with nitrogen 3 times then heated at 100° C. for 6 h. Once cooled, the reaction mixture was diluted with EA (40 mL), washed with water (3×40 mL) and brine (40 mL). The organic phase was dried over MgSO4, filtered and concentrated in vacuo to afford a brown-green solid. The crude product was purified by chromatography (0-50% EA in hexanes) to afford 270 mg (37%) of 4-(5-(4-(heptyloxy)phenyl)thiazol-2-yl)benzaldehyde as an iridescent yellow solid. LCMS-ESI (m/z) calculated for C23H25NO2S: 379.5. found 380.0 [M+H]+, tR=2.99 min. (Method 8).

Aufarbeitung

  1. customThe reaction mixture was evacuated
  2. custompurged with nitrogen 3 times
  3. temperatureOnce cooled
  4. additionthe reaction mixture was diluted with EA (40 mL)
  5. washwashed with water (3×40 mL) and brine (40 mL)
  6. dry with materialThe organic phase was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto afford a brown-green solid
  10. customThe crude product was purified by chromatography (0-50% EA in hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-dbcc2249b57e4496a308318ca5485e9d
Quelldatensatz
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09260427B2

Notizen zur Reaktion

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