Methylamine → HCID 54965987, Verbindung

HRID 1429661Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1429661
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[F:16])[CH2:5][N:6]1[CH2:11][CH2:10][C:9](=O)[CH2:8][CH2:7]1.S1C=CC=C1.[CH3:22][NH2:23].[H][H]>[Pd].CO>[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[F:16])[CH2:5][N:6]1[CH2:11][CH2:10][CH:9]([NH:23][CH3:22])[CH2:8][CH2:7]1

Komponenten

7

Edukt 4

HCID 6329MethylamineHCID 8030ThiopheneHCID 23218604HCID 23218604, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 54965987HCID 54965987, VerbindungAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A suspension of D4 (5.4 g, 24 mmol), thiophene solution (4% in diisopropylether; 2 ml), methylamine solution (40% in water, 10 ml) and 10% palladium on carbon (2 g) in methanol (150 ml) were hydrogenated at atmospheric pressure and temperature until 1 eq. (˜600 ml) of hydrogen had been taken up. After this period, the reaction mixture was filtered and the filtrate evaporated in vacuo. The crude product was purified by column chromatography (silica; 5%-10% ammonia in methanol/dichloromethane) to give D5 (4.7 g, 81%). C13H18F2N2 requires 240; Found 241 (MH+)

Aufarbeitung

  1. waitAfter this period
  2. filtrationthe reaction mixture was filtered
  3. customthe filtrate evaporated in vacuo
  4. customThe crude product was purified by column chromatography (silica; 5%-10% ammonia in methanol/dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-8fafb6609754459aa8e53b8264098888
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08940743B2

Notizen zur Reaktion

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