反応 #93842

ord-7c103829d3a646d2a4191b05b82a94e1

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過the reaction mixture was filtered
  2. 2
    その他the solid recrystallized from ethyl acetate
  3. 3
    その他recrystallized from acetonitrile
  4. 4
    洗浄After washing with ethyl ether
  5. 5
    その他to remove any unreacted material the product
  6. 6
    その他was recrystallized from ethyl alcohol
  7. 7
    洗浄washed with ethyl acetate

実験手順

To a solution of 0.2 mole octadecanoylchloride in 400 ml ethyl ether was added a solution of 32 g (0.31 mole) 3-dimethylamino-1-propanol in 50 ml ethyl ether. After stirring about 2 hours, the reaction mixture was filtered and the solid recrystallized from ethyl acetate. It was converted to the free base, 3-dimethylaminopropyl octadecanoate, with sodium hydroxide and recrystallized from acetonitrile. A mixture of 18.3 g (0.049 mole) of this amine and 16.2 g (0.049 mole) of 1-bromooctadecane was heated in an oven at 100° C. for 7 hours. After washing with ethyl ether to remove any unreacted material the product was recrystallized from ethyl alcohol and washed with ethyl acetate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04128485uspto-grants-1978_12