تفاعل #1218

ord-6f171f3959e24ce6acc5b2cc1ccb94f6

المتفاعلات

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA 500-ml flask equipped with a stirrer
  2. 2
    workup.ADDITIONwere added dropwise over 3 hours
  3. 3
    workup.STIRRINGStirring
  4. 4
    workup.DISTILLATIONBenzyl alcohol was distilled off under reduced pressure
  5. 5
    workup.ADDITIONthe residue was charged into a 500-ml autoclave, to which 300 ml of ethanol and 10 g of 5% Pd/C
  6. 6
    workup.ADDITIONwere added
  7. 7
    أخرىfor 48 hours
  8. 8
    أخرىat room temperature
  9. 9
    أخرىAfter the catalyst was separated by filtration
  10. 10
    تركيزthe filtrate was concentrated under reduced pressure
  11. 11
    أخرىthe residue was recrystallized from hexane

الإجراء التجريبي

A 500-ml flask equipped with a stirrer was charged with 160 g (1.5 mol) of benzylamine, to which 29 g (0.11 mol) of 1,2-epoxyoctadecane were added dropwise over 3 hours while stirring at 100° C. Stirring was conducted further for 12 hours at 100° C. Benzyl alcohol was distilled off under reduced pressure, and the residue was charged into a 500-ml autoclave, to which 300 ml of ethanol and 10 g of 5% Pd/C were added to conduct hydrogenolysis for 48 hours at room temperature under a hydrogen pressure of 5 atm. After the catalyst was separated by filtration, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from hexane, thereby obtaining 26.1 g (yield: 83%) of the title compound (IIh-7).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723497uspto-grants-1998_03