Hydrochloric Acid → Ethyl (4-chlorobenzyl)carbamate

HRID 495625

Reaktionsgleichung

Reaktionsgleichung von HRID 495625
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[CH:4][CH:3]=1.Cl[C:11]([O:13][CH2:14][CH3:15])=[O:12].Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH:7][C:11](=[O:12])[O:13][CH2:14][CH3:15])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 660364-Chlorobenzylamine

Produkt 1

HCID 874364Ethyl (4-chlorobenzyl)carbamateAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

4-Chlorobenzylamine (1.0556 g) was dissolved in pyridine (5 ml), and to the solution was added dropwise ethyl chloroformate.(0.855 ml) during 5 minutes under ice-cooling. After the mixture was stirred for 3 hours, 1N hydrochloric acid was added and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title compound (1.562 g, 98%).

Aufarbeitung

  1. temperature(0.855 ml) during 5 minutes under ice-cooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution
  4. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8537c4556af84daa82eae7dfe7af07d9
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06939887B2

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