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Water → HCID 15540300, Verbindung

HRID 393143
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 393143
[F:1][C:2]([F:16])([F:15])[C:3]1[C:8]([CH:9]([NH:13][CH3:14])[CH:10]([CH3:12])[CH3:11])=[CH:7][N:6]=[CH:5][N:4]=1.C(=O)([O-])[O-].[K+].[K+].[C:23]1([CH2:29][C:30](Cl)=[O:31])[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.O>C(#N)C>[CH3:14][N:13]([CH:9]([C:8]1[C:3]([C:2]([F:1])([F:15])[F:16])=[N:4][CH:5]=[N:6][CH:7]=1)[CH:10]([CH3:12])[CH3:11])[C:30](=[O:31])[CH2:29][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 7679Phenylacetyl chlorideHCID 11430Potassium CarbonateHCID 22648743HCID 22648743, Verbindung

Produkt 1

HCID 15540300HCID 15540300, VerbindungAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342
Acetonitrile
Lösungsmittel

Versuchsvorschrift

6 g (26 mmol) of 4-trifluoromethyl-5-[1-(N-methylamino)-2-methylpropyl]pyrimidine and 3.6 g (26 mmol) of potassium carbonate were dissolved in 150 ml of acetonitrile, and 4 g (26 mmol) of phenylacetyl chloride was dropwise added, followed by stirring at room temperature for 3 hours. To the reaction solution, 200 ml of water was added, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and the obtained crude crystals were washed with n-hexane to obtain 7.7 g (yield: 85%) of N-methyl-N-[2-methyl-1-(4-trifluoromethylpyrimidin-5-yl)propyl]phenylacetamide as colorless transparent crystals (melting point: 106-109° C.).

Aufarbeitung

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe obtained organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationEthyl acetate was distilled off under reduced pressure
  5. customthe obtained crude crystals
  6. washwere washed with n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-0e1f101c4adf4ddcbc3652a2021644cd
Quelldatensatz
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06806230B1

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