HRID387663

反应详情

EQUATION

反应方程式

HRID 387663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customclose to 20° C.
  2. waitthe stirring is continued for 30 min
  3. customThe two phases are separated
  4. customthe organic phase is dried
  5. additionAdded to the solution
  6. customobtained
  7. stirringThe reaction mixture is stirred for 15 h at a temperature
  8. customclose to 20° C
  9. customThe organic phase is decanted
  10. customseparated from the aqueous phase
  11. washthen washed successively with 15 cm3 of distilled water and 15 cm3 of a saturated solution of sodium chloride
  12. customThe organic phase is dried
  13. concentrationthen concentrated
  14. customa rotary evaporator under reduced pressure (5 kPa)