Toluene → N-Cyanoacetylethylcarbamate

HRID 68537

Reaktionsgleichung

Reaktionsgleichung von HRID 68537
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].[NH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C1(C)C=CC=CC=1.P(Cl)(Cl)(Cl)=O>O.CN(C=O)C>[C:1]([CH2:3][C:4]([NH:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[O:6])#[N:2]

Komponenten

7

Edukt 4

HCID 1140TolueneHCID 5641Carbamic acid, ethyl esterHCID 9740Cyanoacetic acidHCID 24813Phosphorus oxychloride

Produkt 1

HCID 23112N-CyanoacetylethylcarbamateAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

2-cyanoacetic acid (85 g, 1 mol) and ethyl aminoformate (89 g, 1 mol) were added to toluene (500 mL). To the mixture was slowly added phosphorus oxychloride (45 mL, 0.5 mol), and then added DMF (5 mL). The reaction was conducted at 70° C. for 2 h. After cooling, water (500 mL) was added to the reaction solution to quench phosphorus oxychloride. The reaction is filtered by suction. The filtered cake was washed with ethyl ether and dried to produce a white solid (104 g) in a yield of 67%.

Aufarbeitung

  1. temperatureAfter cooling
  2. customto quench phosphorus oxychloride
  3. filtrationThe reaction is filtered by suction
  4. washThe filtered cake was washed with ethyl ether
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-710c1d615b944b7f9adc6d68cc7a8ce0
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822465B2

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