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Lithium Hexamethyldisilazide → 2-Propen-1-yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}carbamate

HRID 1961750
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1961750
[CH2:1]([O:4][C:5]([NH:7][C:8]1[C:9]([F:18])=[C:10]([CH:15]=[CH:16][CH:17]=1)[C:11]([O:13]C)=O)=[O:6])[CH:2]=[CH2:3].[Li+].[CH3:20][Si]([N-][Si](C)(C)C)(C)C.[Cl-:29].[N:30]1[CH:35]=[CH:34][CH:33]=[N:32][CH:31]=1>C1COCC1>[Cl:29][C:31]1[N:32]=[C:33]([CH2:20][C:11]([C:10]2[C:9]([F:18])=[C:8]([NH:7][C:5](=[O:6])[O:4][CH2:1][CH:2]=[CH2:3])[CH:17]=[CH:16][CH:15]=2)=[O:13])[CH:34]=[CH:35][N:30]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 2733832Lithium HexamethyldisilazideHCID 22046915Pyrimidine chlorideHCID 57989974Methyl 3-(allyloxycarbonylamino)-2-fluorobenzoate

Produkt 1

HCID 579899922-Propen-1-yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of methyl 3-(allyloxycarbonylamino)-2-fluorobenzoate (86.7 g, 342 mmol, 1 eq) in dry THF (500 mL) at −10° C., LiHMDS (1M in THF, 1198 mmol, 1198 mL, 3.5 eq) was added dropwise and the solution was allowed to stir for 1 h at 0° C. A solution of pyrimidine chloride (48.0 g, 376 mmol, 1.2 eq) in THF (200 mL) was then added dropwise to the solution of ester and base at 0° C. over 20 min. The solution was allowed to stir 1 h at rt. TLC showed the reaction was complete. The reaction was quenched by addition of the saturated aqueous NH4Cl (800 mL) at 0° C. The reaction mixture was extracted with EtOAc (1 L×3). The combined organic layers were washed with water and brine successively, dried over Na2SO4, filtered and concentrated under reduced pressure to give the crude product, which was purified by flash column on silica gel, rinsing with DCM. This solution was concentrated to obtain a solid. The orange solid was triturated with a small amount of EtOAc and filtered, rinsing with diethyl ether to give the product (240.1 g, 67.0%, three batches combined). 1H NMR (400 MHz, DMSO-d6) δ ppm 13.70 (s, 1H), 8.52 (dd, J=0.8, 4.8 Hz, 0.3H), 8.34 (dd, J=0.8, 5.2 Hz, 1H), 8.27 (s, 0.4H), 8.10 (s, 1H), 7.47 (t, J=8.0 Hz, 1.4H), 7.22-7.12 (m, 1.8H), 6.96 (s, 1.4H), 6.85 (d, J=4.2 Hz, 1H), 6.07 (s, 1H), 5.97-5.86 (m, 1.4H), 5.32 (d, J=15.6 Hz, 1.4H), 5.24 (d, J=6.4 Hz, 1.4H), 4.64 (d, J=6.0 Hz, 2.8H), 4.38 (d, J=2.8 Hz, 0.8H).

Aufarbeitung

  1. stirringto stir 1 h at rt
  2. customThe reaction was quenched by addition of the saturated aqueous NH4Cl (800 mL) at 0° C
  3. extractionThe reaction mixture was extracted with EtOAc (1 L×3)
  4. washThe combined organic layers were washed with water and brine successively
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d821f26aa47b4e02ae0e9e25720cd551
Quelldatensatz
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08415345B2

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