Reaktion #4208

ord-b9d7e217a7e7454187283988eab03121

Reaktionsgleichung

O=C(Cl)CCl
chloroacetyl chloride
O=C([O-])O.[K+]
potassium bicarbonate
Nc1ccc(OCc2ccccc2)c(OCc2ccccc2)c1
3,4-dibenzyloxyaniline
O=C(Cl)CCl
chloroacetyl chloride
O=C(CCl)Nc1ccc(OCc2ccccc2)c(OCc2ccccc2)c1
2-Chloro-N-[3,4-bis(phenylmethoxy)phenyl]acetamide

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile maintaining the pH at 6.5
  2. 2
    workup.WAITWhen the pH remained constant for 15 minutes
  3. 3
    Sonstigethe acetonitrile was evaporated
  4. 4
    Filtrationthe resulting aqueous solution was filtered
  5. 5
    WaschenThe precipitate was washed thoroughly with water
  6. 6
    Sonstigeto yield
  7. 7
    Trocknenupon drying in vacuo, 8.98 g of the title compound

Vorschrift

To 7.7 g (25 mmol) of 3,4-dibenzyloxyaniline in 50 ml of 1:1 acetonitrile/water at 0° C. was added chloroacetyl chloride (3.0 ml) while keeping the pH at 6.5 with saturated aqueous potassium bicarbonate. When the pH remained constant for 15 minutes, an additional 3 ml of chloroacetyl chloride was added in small portions while maintaining the pH at 6.5. When the pH remained constant for 15 minutes, the acetonitrile was evaporated, and the resulting aqueous solution was filtered. The precipitate was washed thoroughly with water to yield, upon drying in vacuo, 8.98 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04723002uspto-grants-1988_02