反应 #1178396

ord-3172d48492684866a26c03fcf649f011

反应方程式

Cl
HCl
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCNCC
diethyl amine
BrCc1ccc(Br)cc1
p-bromobenzyl bromide
CCN(CC)Cc1ccc(Br)cc1
(p-bromobenzyl)diethyl amine
收率 74.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added
  2. 2
    萃取The mixture was extracted with 100 ml diethyl ether for three times
  3. 3
    干燥The diethyl ether solution was dried with anhydrous magnesium sulfate over night
  4. 4
    其他the magnesium sulfate was removed by filtration
  5. 5
    其他Diethyl ether was evaporated
  6. 6
    其他the raw product was purified by a silica gel column

实验过程

Into a 500 ml round-bottomed flask were added 150 ml THF, 5 ml water, 2.2 g potassium carbonate, 6 ml diethyl amine, and 5 g p-bromobenzyl bromide. The resultant mixture was refluxed for 12 h. The mixture was then cooled to room temperature, into which 6 ml concentrated HCl was added, followed by the addition of 150 ml water. The mixture was extracted with 100 ml diethyl ether for three times. The diethyl ether solution was dried with anhydrous magnesium sulfate over night and then the magnesium sulfate was removed by filtration. Diethyl ether was evaporated and the raw product was purified by a silica gel column using hexane/chloroform mixture (1:1 by volume) as the eluent. (p-bromobenzyl)diethyl amine (BBDA) was obtained in 74% yield (3.6 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08129111B2uspto-grants-2012_03