反応 #413261
ord-40021112fc3b451e884eb49b0a41fcf8
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度heated to 150°-165° for 22 hours
- 2workup.DISTILLATIONExcess γ-butyrolactone was then distilled off at reduced pressure (80°/2 mm)
- 3workup.ADDITIONThe light brown residue was poured into a crystallization dish where it
- 4ろ過filtered
- 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°.