تفاعل #474845

ord-e628a63ecdb64a70bdec3918cb9c8c45

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىclose to 20° C.
  2. 2
    workup.WAITthe stirring is continued for 30 min
  3. 3
    أخرىThe two phases are separated
  4. 4
    أخرىthe organic phase is dried
  5. 5
    workup.ADDITIONAdded to the solution
  6. 6
    أخرىobtained
  7. 7
    workup.STIRRINGThe reaction mixture is stirred for 15 h at a temperature
  8. 8
    أخرىclose to 20° C
  9. 9
    أخرىThe organic phase is decanted
  10. 10
    أخرىseparated from the aqueous phase
  11. 11
    غسيلthen washed successively with 15 cm3 of distilled water and 15 cm3 of a saturated solution of sodium chloride
  12. 12
    أخرىThe organic phase is dried
  13. 13
    تركيزthen concentrated
  14. 14
    أخرىa rotary evaporator under reduced pressure (5 kPa)

الإجراء التجريبي

Added to a suspension of 1 g of 2-bromo-4-trifluoromethylphenethylamine hydrocloride in 25 cm3 of dichloroethane and under an inert atmosphere is 0.5 cm3 of triethylamine. After stirring for 30 min at a temperature close to 20° C., 5 cm3 of distilled water are added and the stirring is continued for 30 min. The two phases are separated and the organic phase is dried. Added to the solution obtained are successively 375 mg of 4-heptanone and 970 mg of sodium triacetoxyborohydride. The reaction mixture is stirred for 15 h at a temperature close to 20° C. 20 cm3 of a saturated solution of sodium hydrogen carbonate are then added to the reaction medium. The organic phase is decanted and separated from the aqueous phase then washed successively with 15 cm3 of distilled water and 15 cm3 of a saturated solution of sodium chloride. The organic phase is dried then concentrated using a rotary evaporator under reduced pressure (5 kPa). 1.16 g of N-[2-(2-bromo-4-trifluoromethylphenyl)ethyl]heptan-4-amine are obtained in the form of a colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08372864B2uspto-grants-2013_02