Dimethylcarbamoyl Chloride → Urea, N,N-dimethyl-N-2-propynyl- (9CI)

HRID 600184Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 600184
[CH3:1][N:2]([CH3:6])[C:3](Cl)=[O:4].[CH2:7]([NH2:10])[C:8]#[CH:9].CN(C1C=CC=CN=1)C>N1C=CC=CC=1.C(OCC)(=O)C>[CH3:1][N:2]([CH3:6])[C:3]([NH:10][CH2:7][C:8]#[CH:9])=[O:4]

Komponenten

6

Edukt 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 218852-DimethylaminopyridineHCID 239041Propargylamine

Produkt 1

HCID 44190381Urea, N,N-dimethyl-N-2-propynyl- (9CI)

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Dimethyl carbamylchloride (0.84 mL, 9.1 μmmol) was added to a stirred solution of propargylamine (0.62 mL, 9.1 mmol) and dimethylaminopyridine (22 mg, 0.18 mmol) in pyridine (5 mL) at room temperature. The resulting suspension was stirred at ambient temperature for approximately 15 h. The reaction mixture was diluted with ethyl acetate and washed successively with 1N HCl and brine. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound (i-3), which was used without further purification.

Aufarbeitung

  1. washwashed successively with 1N HCl and brine
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e73d60aa1093461792ddc3b483d53425
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07901893B2

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