Reaktion #2985

ord-23a827758ec74998ac781f9b6412b1c4

Reaktionsgleichung

Cl
hydrochloric acid
O=C([O-])[O-].[K+].[K+]
potassium carbonate
COc1ccc2cccc(CCCN)c2c1.Cl
3-(7-methoxy-1-naphthyl)propylamine hydrochloride
CC(=O)Cl
acetyl chloride
COc1ccc2cccc(CCCNC(C)=O)c2c1
N-[3-(7-METHOXY-1-NAPHTHYL)PROPYL]ACETAMIDE

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe amine precipitates
  2. 2
    workup.ADDITIONThereafter, 50 cm3 of chloroform are added
  3. 3
    workup.WAITThe medium is left
  4. 4
    workup.STIRRINGstirred for 15 minutes
  5. 5
    ExtraktionThe aqueous phase is extracted with 3 times 50 cm3 of chloroform
  6. 6
    WaschenThe organic phases are washed with water
  7. 7
    Trocknendried over calcium chloride
  8. 8
    Sonstigeevaporated
  9. 9
    SonstigePurification of the products
  10. 10
    Sonstigeis performed either by recrystallization or by column chromatography

Vorschrift

After 0.005 mol (equivalent to 1.26 g) of 3-(7-methoxy-1-naphthyl)propylamine hydrochloride has been dissolved in 20 cm3 of water, 0.015 mol of potassium carbonate is added. The amine precipitates. Thereafter, 50 cm3 of chloroform are added and 0.010 mol of acetyl chloride is added dropwise. The medium is left stirring for 2 hours. It is acidified with 2N of hydrochloric acid and then stirred for 15 minutes. The aqueous phase is extracted with 3 times 50 cm3 of chloroform. The organic phases are washed with water, dried over calcium chloride and evaporated. Purification of the products is performed either by recrystallization or by column chromatography.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05731352uspto-grants-1998_03