Morpholine → 2,6-Difluoro-4-(morpholin-4-yl)benzonitrile

HRID 2054890

Reaktionsgleichung

Reaktionsgleichung von HRID 2054890
[F:1][C:2]1[CH:9]=[C:8](F)[CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5].[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.C(N(CC)C(C)C)(C)C>CO.O>[F:1][C:2]1[CH:9]=[C:8]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5]

Komponenten

6

Edukt 3

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 7371772,4,6-Trifluorobenzonitrile

Produkt 1

HCID 115286822,6-Difluoro-4-(morpholin-4-yl)benzonitrileAusbeute 68,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of 1.0 g (6.37 mmol) of 2,4,6-trifluorobenzonitrile in MeOH (25 mL) was added 0.6 mL (6.9 mmol) of morpholine and 1.2 mL (6.7 mmol) of N,N-diisopropylethylamine. The mixture was heated to 50° C. for 6 h then cooled to room temperature and diluted with H2O which caused a solid to precipitate from solution. The white solid was collected by filtration, washed with H2O and dried under vacuum to provide 0.98 g (68%) of 2,6-difluoro-4-morpholin-4-yl-benzonitrile as a white solid.

Aufarbeitung

  1. temperaturethen cooled to room temperature
  2. customto precipitate from solution
  3. filtrationThe white solid was collected by filtration
  4. washwashed with H2O
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f2505ceb71034e728e2a4655b9a619a7
Quelldatensatz
uspto-grants-2008_02
Patentnummer
US07329764B2

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