반응 #2985

ord-23a827758ec74998ac781f9b6412b1c4

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The 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
    추출The aqueous phase is extracted with 3 times 50 cm3 of chloroform
  6. 6
    세척The organic phases are washed with water
  7. 7
    건조dried over calcium chloride
  8. 8
    기타evaporated
  9. 9
    기타Purification of the products
  10. 10
    기타is performed either by recrystallization or by column chromatography

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731352uspto-grants-1998_03