反応 #413261

ord-40021112fc3b451e884eb49b0a41fcf8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated to 150°-165° for 22 hours
  2. 2
    workup.DISTILLATIONExcess γ-butyrolactone was then distilled off at reduced pressure (80°/2 mm)
  3. 3
    workup.ADDITIONThe light brown residue was poured into a crystallization dish where it
  4. 4
    ろ過filtered
  5. 5
    洗浄the tan powder was washed with chloroform

実験手順

11.62 g (0.1 M) of 1,6-diaminohexane and 21.66 g (0.25 M) of γ-butyrolactone were mixed and heated to 150°-165° for 22 hours. Excess γ-butyrolactone was then distilled off at reduced pressure (80°/2 mm). The light brown residue was poured into a crystallization dish where it immediately solidified. The solid was taken in chloroform, powdered, filtered and the tan powder was washed with chloroform. Yield 22.0 g (87%); melting point 101°-103°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04444762uspto-grants-1984_04