Benzyl isocyanate → ethyl 2-(1-Methyl-2-(benzylcarbamoyl)hydrazinyl)acetate

HRID 576875Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 576875
[CH3:1][N:2]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH2:3].[CH2:10]([N:17]=[C:18]=[O:19])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>O1CCCC1.C(OCC)(=O)C>[CH3:1][N:2]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH:3][C:18](=[O:19])[NH:17][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

Komponenten

5

Edukt 2

HCID 76639Benzyl isocyanateHCID 20288078Ethyl 2-(1-methylhydrazinyl)acetate

Produkt 1

HCID 66977957ethyl 2-(1-Methyl-2-(benzylcarbamoyl)hydrazinyl)acetateAusbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of ethyl 2-(1-methylhydrazinyl)acetate (Compound XL-1) 10 ml (76 mmol) in tetrahydrofuran 40 ml, benzyl isocyanate 11.1 g (83.3 mmol) was added at 0° C. and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate 150 ml and washed with water 75 ml and brine 75 ml. The organic phase was dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to obtain the title compound 15.2 g (76%).

Aufarbeitung

  1. washwashed with water 75 ml and brine 75 ml
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e456841d45a84c60b5e7cea3ed743214
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09040531B2

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