3,3-Dimethylbutylamine → HCID 178444765, Verbindung

HRID 1695943

Reaktionsgleichung

Reaktionsgleichung von HRID 1695943
[O:1]1[CH2:6][CH2:5][N:4]([CH2:7][CH2:8][NH:9][C:10]2[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:11]=2[CH:12]=O)[CH2:3][CH2:2]1.[CH3:19][C:20]([CH3:25])([CH3:24])[CH2:21][CH2:22][NH2:23].[O-]S([O-])(=O)=O.[Mg+2]>C1(C)C=CC=CC=1>[CH3:19][C:20]([CH3:25])([CH3:24])[CH2:21][CH2:22]/[N:23]=[CH:12]/[C:11]1[CH:14]=[CH:15][CH:16]=[C:17]([F:18])[C:10]=1[NH:9][CH2:8][CH2:7][N:4]1[CH2:5][CH2:6][O:1][CH2:2][CH2:3]1

Komponenten

5

Edukt 3

HCID 197093,3-DimethylbutylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 57774415HCID 57774415, Verbindung

Produkt 1

HCID 178444765HCID 178444765, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

2-(2-Morpholinoethylamino)-3-fluorobenzaldehyde (495 mg, 1.962 mmol), 3,3-dimethylbutan-1-amine (400 μL, 2.973 mmol), and MgSO4 were added to toluene (15 mL) and the reaction stirred in a 70° C. oil bath overnight. The oil bath temperature was raised to 100° C. for 2.5 hours, then heat was removed, solvent and volatiles removed under high vacuum on a rotary evaporator at 35° C. to give 2-((E)-(3,3-dimethylbutylimino)methyl)-6-fluoro-N-(2-morpholinoethyl)benzenamine. The crude material was carried on to the next reaction. FIA: 336.49 (M+1).

Aufarbeitung

  1. temperatureThe oil bath temperature was raised to 100° C. for 2.5 hours
  2. temperatureheat
  3. customwas removed
  4. customsolvent and volatiles removed under high vacuum on a rotary evaporator at 35° C.

Quellen und Nachweise

ORD-Eintrag
ord-f3faa93ca66a43a1bb7ed6934ae20f26
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08163737B2

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