Oxalyl chloride → 4,6-Dimethylbenzothiophene-2,3-dione

참여 물질

반응 단계

To a solution of AlCl3(0.4 g,3.6 mmol) in CH2Cl2 (4 mL) at −20 C under nitrogen were added 3,5-dimethylbenzenethiol (1 g, 7.2 mmol) and oxalyl chloride (0.6 mL, 7.2 mmol) respectively. The solution was warmed to room temperature for 1 hour and was heated to 120 C in a microwave reactor for 15 minutes. The solution was cooled down and was pouled into crashed ice. The solution was extracted with CH2Cl2 and the organic layer was collected. The solution was dried with MgSO4 and was filtered. The filtrate was concentrated and the residue was purified by Combi-Flash with 5% EtOAc in Hexane as the eluent to afford the desirable product 4,6-Dimethyl-benzo[b]thiophene-2,3-dione (500 mg, 35%).

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