Lithium hydride → HCID 178436207, Verbindung

HRID 1732887Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1732887
I.[NH:2]=[C:3]1[NH:7][CH2:6][CH2:5][NH:4]1.[H-].[Li+].[CH2:10]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[C:13]=1[N:19]=[C:20]=[O:21])[CH3:11]>CN(C)C=O>[CH2:10]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[C:13]=1[NH:19][C:20]([N:2]=[C:3]1[NH:7][CH2:6][CH2:5][NH:4]1)=[O:21])[CH3:11]

Komponenten

5

Edukt 3

HCID 62714Lithium hydrideHCID 27364482-Ethyl-6-methylphenyl isocyanateHCID 178506595HCID 178506595, Verbindung

Produkt 1

HCID 178436207HCID 178436207, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

In a manner similar to that previously described, 15.55 grams (0.073 mole) of 2-iminoimidazoline hydroiodide is added dropwise to a dry cooled suspension of 596 milligrams (0.075 mole) of lithium hydride in 30 milliliters of dimethylformamide under an atmosphere of nitrogen. After completion of the addition, the mixture is allowed to warm to room temperature to complete the reaction. Thereafter the mixture is again cooled, a solution of 8.1 grams (0.05 mole) of 2-ethyl-6-methylphenyl isocyanate in 25 milliliters of dry dimethylformamide is added dropwise over a two hour period and thereafter the resulting mixture is stirred overnight while the temperature is allowed to rise to ambient temperatures to obtain a N-(2-ethyl-6-methylphenyl-N'-(2-imidazolidinylidene)urea product. The base product is recovered by procedures similar to that previously described and after recrystallization from methanol-water, a purified base product, m.p. 185°-187° C. is obtained.

Aufarbeitung

  1. temperaturecooled
  2. additionAfter completion of the addition
  3. customthe reaction
  4. temperatureThereafter the mixture is again cooled

Quellen und Nachweise

ORD-Eintrag
ord-727d590dbda04da38ccc9636e9ab8e2a
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04239768

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