Rakı is a traditional alcoholic spirit that distills from grapes/raisins distillate so‐called suma with aniseed (Pimpinella anisum) in the copper pot still distillers. During distillation, middle‐cut fractions are separated and used for Rakı productions. Lately, triple pot still distillations as a new process is also used for production. In this study, effect of distillation numbers on volatile compounds of middle‐cut fraction during the Rakı production was investigated. Minor volatiles were extracted with liquid–liquid extraction method and analyzed with GC‐MS/FID. Major volatiles were analyzed by direct injection with GC‐FID. Odor‐active compounds are also identified by GC‐O technique. While the number of distillations increased, the amount of volatiles from aniseed and suma decreased and the amount of higher alcohols, esters, and aldehydes of middle‐cut fractions are decreased. The highest amount of volatiles based on aniseed are determined as trans‐anethole, estragole, cis‐anethole, and γ‐himachalene. Odor‐active compounds were identified as anethole, estragole, linalool, ethyl‐2‐methyl‐butanote, γ‐himachalene, and p‐anisaldehyde. Practical applications Rakı is produced by distillation of “suma (grape distillate)” with aniseed (Pimpinella anisum) in traditional copper distillers (pot still) having volume of 5.000 liters. Suma is the distillate originating from grapes/raisin that is distilled up to 94.5% v/v alcohol by column still distillation with the purpose of keeping the flavor and smell of grapes. Rakı is a reach product in term of volatile compounds coming from grape distillate and aniseed. Despite of simple (traditional) pot still distillations, triple pot still distillations as a new process is also used in order to improve the quality for Rakı production. While the number of distillations increased, the amount of esters, terpenes, and aldehydes and volatile phenols are decreased. Off‐flavors coming from suma as like pungent, woody, fishy smells are separated with increasing the number of the distillations. So perceptions of odor‐active compounds that is desired become more powerful in triple distillation.