Intercalation behavior of acetylsalicylic acid (ASA) to interlayer of hydrotalcite (HT) was investigated in various organic solvents to synthesize ASA/HT composite. ASA intercalation to the interlayer of HT did not occur in an aprotic solvent like acetone but occurred in a protic solvent like alcohols. In the case of alcohols used for solvent, the intercalation behavior was revealed to depend on the alcohol's type. In the primary alcohol (methanol, ethanol, 1-propanol, 1-butanol, and i-butanol), the acetylsalicylate ions were not intercalated, but the salicylate ions were intercalated into the interlayer of HT because of the complete decomposition of ASA in the solution. Since ASA decomposed partially in the secondary alcohol (2-propanol and 2-butanol), the both acetylsalicylate and salicylate ions were intercalated into the interlayer of HT. On the other hand, the decomposition of ASA was substantially restricted in the tertiary alcohol (tert-butanol) because of the stability of the tertiary alcohol. As a result, the acetylsalicylate ions were found to intercalate into the interlayer of HT over 80 mol% and ASA/HT composite was successfully obtained using tert-butanol as solvent.