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Methylamine → HCID 22648743, Verbindung

HRID 393160
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 393160
Cl[CH:2]([C:6]1[C:7]([C:12]([F:15])([F:14])[F:13])=[N:8][CH:9]=[N:10][CH:11]=1)[CH:3]([CH3:5])[CH3:4].[CH3:16][NH2:17]>C(O)(C)C>[CH3:16][NH:17][CH:2]([C:6]1[C:7]([C:12]([F:15])([F:14])[F:13])=[N:8][CH:9]=[N:10][CH:11]=1)[CH:3]([CH3:5])[CH3:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 22648742HCID 22648742, Verbindung

Produkt 1

HCID 22648743HCID 22648743, VerbindungAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

4.5 g (19 mmol) of 5-(1-chloro-2-methylpropyl)-4-trifluoromethylpyrimidine was dissolved in 50 ml of isopropyl alcohol, and 10 ml (161 mmol) of a 50% methylamine aqueous solution was added, followed by stirring at room temperature for 8 hours. The solvent was distilled off under reduced pressure, and 100 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 to obtain 3.4 g (yield: 77%) of 5-(1-(N-methylamino)-2-methylpropyl]-4-trifluoromethylpyrimidine as slightly yellow liquid (refractive index nD20: 1.4529).

Aufarbeitung

  1. distillationThe solvent was distilled off under reduced pressure, and 100 ml of water
  2. additionwas added
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe obtained organic layer was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationEthyl acetate was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-91087a98e80d475aa2b090dd5f3a38d5
Quelldatensatz
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06806230B1

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