An innovative process combining roasting and tempering was proposed to promote puffing and mechanical dehulling of jicaro seeds. Roasting was performed at three temperatures (120 °C, 140 °C, and 160 °C) and for six residence times (80–180 s). A previous seed tempering was performed at 15% moisture content for 24 h, by spraying the seeds with an amount of water calculated to reach the final moisture content of 15%. The following parameters were monitored as a function of time to optimize the roasting operation: percentage of open seeds, whiteness of cotyledons, and content of two volatile compounds, 2,5-dimethylpyrazine and ethyl-2-methylbutyrate which are considered as the key jicaro note. The optimal roasting was achieved at 160 °C for 150 s with 90% open seeds. The optimal mechanical dehulling was achieved after tempering the roasted seed at 10% moisture content with a yield of 75%. The lightness evolution followed a zero-order kinetic with an activation energy of 103 kJ mol-1. Ethyl-2-methylbutyrate and 2,5-dimethylpyrazine increased with the temperature and period of roasting.