Реакция #2985

ord-23a827758ec74998ac781f9b6412b1c4

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe 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
    ЭкстракцияThe aqueous phase is extracted with 3 times 50 cm3 of chloroform
  6. 6
    ПромывкаThe organic phases are washed with water
  7. 7
    Сушкаdried over calcium chloride
  8. 8
    Другоеevaporated
  9. 9
    ДругоеPurification of the products
  10. 10
    Другоеis performed either by recrystallization or by column chromatography

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05731352uspto-grants-1998_03