反应详情

温度

113 °C

To 5-amino-2,2,4-trimethylcyclopentylmethylamine (127.72 g, 0.819 mol) in xylene (525 ml) at 122° C. was added with stirring 2,2,6-trimethyl-1,3-dioxen-4-one (232.51 g, 1.637 mol) in xylene (525 mol) over 10 minutes, during which the temperature decreased to 104° C. After heating to 113° C. over 5 minutes, vigorous effervescence and distillation of acetone (through a Vigreux column) commenced. Pot temperature was increased to 127° C. over 5 minutes and to 140° C. over a further 30 minutes, with collection of acetone distillate. After cooling to 39° C., dichloromethane was added, and removal of solvent and drying (93° C./100 Pa) gave 1-acetoacetamido-2-acetoacetamidomethyl-3,3,5-trimethylcyclopentane (237.03 g, 89%), (AAMTCP), which was crushed to a light yellow powder, mp 94-114° C. (mixture of stereoisomers), and identified by 1H-NMR, 13C-NMR, FT-IR and Raman spectra.

1. customdecreased to 104° C
2. distillationvigorous effervescence and distillation of acetone (through a Vigreux column)
3. temperaturePot temperature was increased to 127° C. over 5 minutes and to 140° C. over a further 30 minutes, with collection of acetone distillate
4. temperatureAfter cooling to 39° C.
5. additiondichloromethane was added
6. customremoval of solvent
7. customdrying (93° C./100 Pa)