反应详情

A solution of the N-formyl-N-[2-(dimethylamino)-cyclohexanediamine (4 g.; 0.0235 mole) in 50 ml. of ether was added during 5 minutes to a solution of LAH (4 g.) in 250 ml. of ether and refluxed 17 hours. It was cooled in ice, and decomposed in succession with 4 ml. of H2O, 4 ml. of 15% NaOH, 12 ml. of H2O, stirred 1 hour at room temperature and filtered. The cake was washed with ether, and the ether was distilled. The titled amine (B) residue was distilled at 14 mm, b.p. 86°-87°, 3 g. (82% yield). ir NH 3680 v.w., 3320; CH 2940, 2820; N-alkyl 2780; CH 1475, 1450; C-N/other 1270, 1155, 1145, 1125, 1060, 1045, 1005, 870, 805, 775. nmr in CDCl3 (60 MHz) was in accord. Mass spectrum M+ 156.

1. temperatureIt was cooled in ice
2. filtrationfiltered
3. washThe cake was washed with ether
4. distillationthe ether was distilled
5. distillationThe titled amine (B) residue was distilled at 14 mm, b.p. 86°-87°, 3 g