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Diisopropylamine → (4,6-dichloropyrimidin-5-yl)[1-methyl-5-(4-methylphenyl)-1H-pyrazol-4-yl]methanol

HRID 72698
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 72698
C([Li])CCC.C(NC(C)C)(C)C.[Cl:13][C:14]1[CH:19]=[C:18]([Cl:20])[N:17]=[CH:16][N:15]=1.[CH3:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]2[N:32]([CH3:33])[N:31]=[CH:30][C:29]=2[CH:34]=[O:35])=[CH:24][CH:23]=1>O1CCCC1>[Cl:13][C:14]1[C:19]([CH:34]([C:29]2[CH:30]=[N:31][N:32]([CH3:33])[C:28]=2[C:25]2[CH:26]=[CH:27][C:22]([CH3:21])=[CH:23][CH:24]=2)[OH:35])=[C:18]([Cl:20])[N:17]=[CH:16][N:15]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 7912DiisopropylamineHCID 709434,6-DichloropyrimidineHCID 838192491-Methyl-5-(p-tolyl)-1H-pyrazole-4-carbaldehydeHCID 178418339Butyllithium

Produkt 1

HCID 86712557(4,6-dichloropyrimidin-5-yl)[1-methyl-5-(4-methylphenyl)-1H-pyrazol-4-yl]methanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel
3×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

n-Butyllithium (2.5 M in hexanes, 240 mL, 0.60 mol) was added drop-wise to a solution of diisopropylamine (85.2 mL, 0.60 mol) in tetrahydrofuran (600 mL) at −78° C. After the reaction had stirred for 30 minutes at −78° C., a solution of 4,6-dichloropyrimidine (89.4 g, 0.600 mol) in tetrahydrofuran (600 mL) was added drop-wise at about −90° C., and stirring was continued for 1 hour. To this mixture was added drop-wise a solution of 5-(4-methylphenyl)-1-methyl-1H-pyrazole-4-carbaldehyde (C3) (60.0 g, 300 mmol) in tetrahydrofuran (600 mL) at about −90° C. After completion of the addition, the reaction mixture was stirred at this temperature for 2 hours. The reaction mixture was quenched with acetic acid (60 g); the mixture was warmed to room temperature, and then concentrated under reduced pressure to remove tetrahydrofuran. The residue was dissolved in ethyl acetate (2 L) and washed with saturated aqueous sodium bicarbonate solution (1 L). The organic layer was washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, and concentrated in vacuo. Recrystallization from ethyl acetate yielded the product as a white solid. Yield: 82.0 g, 235 mmol, 78%. 1H NMR (400 MHz, CDCl3) δ 2.39 (s, 3H), 3.72 (s, 3H), 6.26 (s, 1H), 7.17 (br AB quartet, JAB=8 Hz, ΔνAB=32 Hz, 4H), 7.66 (s, 1H), 8.55 (s, 1H).

Aufarbeitung

  1. stirringstirring
  2. waitwas continued for 1 hour
  3. additionAfter completion of the addition
  4. stirringthe reaction mixture was stirred at this temperature for 2 hours
  5. customThe reaction mixture was quenched with acetic acid (60 g)
  6. temperaturethe mixture was warmed to room temperature
  7. concentrationconcentrated under reduced pressure
  8. customto remove tetrahydrofuran
  9. dissolutionThe residue was dissolved in ethyl acetate (2 L)
  10. washwashed with saturated aqueous sodium bicarbonate solution (1 L)
  11. washThe organic layer was washed with saturated aqueous sodium chloride solution
  12. dry with materialdried over sodium sulfate
  13. concentrationconcentrated in vacuo
  14. customRecrystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-b508eddb524f46008fe02f70caf89b18
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08829010B2

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