Aluminum chloride (49.68 g, 372.60 mmol) and 2,6-dichloro toluene (50.00 g, 310.50 mmol) were added to the single-mouth flask under stir at room temperature. Then acetyl chloride (26.81 g, 341.60 mmol) is added dropwise. The reaction was heated to 40°C for 2 hours, and the reaction of the raw materials was monitored by TLC to be complete. Pour the system slowly into ice water (500mL), dilute hydrochloric acid solution(1M, 30mL) acidified, extracted with dichloromethane (150mL x 3). It was dried over anhydrous sodium sulfate and concentrated to obtain 2,4-Dichloro-3-Methylacetophenone as a colorless oil with a yield of 95%.