Abstract A green route fast synthesis of triacetylphloroglucinol analogue has been described in detail. This process efficiently achieved by a Friedel-Craft acylation in a one-pot method using phloroglucinol and appropriate acetic anhydride or acyl chloride as acylation agents in the presence of biodegradable catalyst methanesulfonic acid under solvent-free condition. This novel protocol clearly demonstrated green chemistry concept in term of simplicity, good yields and environment-friendly conditions.