反应详情

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

1. temperatureis heated to 120° C. in a microwave reactor for 15 minutes
2. temperatureThe solution is cooled
3. additionis poured
4. custominto crushed ice
5. extractionThe solution is extracted with CH2Cl2
6. customthe organic layer is collected
7. dry with materialThe solution is dried with MgSO4
8. filtrationis filtered
9. concentrationThe filtrate is concentrated
10. customthe residue is purified by flash chromatography with 5% EtOAc in Hexane as the eluent