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

HRID 641144Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 641144
[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 mmol) was added to a stirred solution of propargylamine (0.62 mL, 0.1 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-44c52bb23c9f4c6989f513e2200b832e
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07696177B2

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