Reaktion #51478

ord-2a56fa04ecc14d22a9f17835b82ef9ba

Reaktionsgleichung

O=C(CCl)NCCc1ccc2c(c1)OCO2
2-chloro-N-[2-(1,3-benzodioxol-5-yl)ethyl]acetamide
NCCCO
3-aminopropanol
O=C(CNCCCO)NCCc1ccc2c(c1)OCO2
2-[(3-hydroxypropyl)amino]-N-[2-(1,3-benzodioxol-5-yl)ethyl]acetamide
Ausbeute 82.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter heating
  2. 2
    Sonstigethe reaction in an oil bath at 60° C. for 1 day
  3. 3
    Sonstigethe reaction was partitioned with ethyl acetate and water
  4. 4
    SonstigeThe organic layer was separated
  5. 5
    Waschenwashed with brine
  6. 6
    Trocknendried (Na2SO4)
  7. 7
    Sonstigethe solvent was removed in vacuo

Vorschrift

To 2-chloro-N-[2-(1,3-benzodioxol-5-yl)ethyl]acetamide (0.45 g, 1.9 mmol) in ethanol (10 mL) was added 3-aminopropanol (0.72 mL, 9.4 mmol) (a compound of formula (Y9)). After heating the reaction in an oil bath at 60° C. for 1 day, the reaction was partitioned with ethyl acetate and water. The organic layer was separated, washed with brine, dried (Na2SO4), and the solvent was removed in vacuo to give 0.44 g of 2-[(3-hydroxypropyl)amino]-N-[2-(1,3-benzodioxol-5-yl)ethyl]acetamide, a compound of formula (Y10).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06849739B2uspto-grants-2005_02