A kind of preparation method of 2-methyl-1,2,3,9-tetrahydrobenzo[b]pyrrole[1,4]-thiazine-1,3-dione compound

[0039] Take 1.3g (0.01mol) of o-aminothiophenol, 1.1g (0.01mol) of N-methylmaleimide, and 0.19g (0.001mol) of cuprous iodide, and add them to a 100mL round-bottomed flask. Oxygen, then add N,N-dimethylformamide (DMF) 10mL, keep 120°C for 8 hours, after the reaction is complete, add 30mL of water, stir for 5 minutes, extract with ethyl acetate 50mL×3, dry the organic phase, and use 95% ethanol Crystallization gave 1.22 g of yellow solid 2-methyl-1,2,3,9-tetrahydrobenzo[b]pyrrole[1,4]-thiazine-1,3-dione, yield 52.6%, mp: 236~238℃.

[0041]Take 5.0g (0.04mol) of o-aminothiophenol, 8.9g (0.08mol) of N-methylmaleimide, and 7.6g (0.04mol) of cuprous iodide, and add them to a 100mL round-bottomed flask. Oxygen, then add 60mL of N,N-dimethylacetamide (DMA), keep at 120°C for 12h, after the reaction is complete, add 100mL of water, stir for 5 minutes, extract with 100mL×3 ethyl acetate, dry the organic phase, and use 95% ethanol Crystallization gave 7.8 g of yellow solid 2-methyl-1,2,3,9-tetrahydrobenzo[b]pyrrole[1,4]-thiazine-1,3-dione, yield 85.3%, mp: 237~240℃.

[0043] Take 5.0g (0.04mol) of o-aminothiophenol, 4.4g (0.04mol) of N-methylmaleimide, and 3.8g (0.02mol) of cuprous iodide, and add them to a 100mL round-bottomed flask. Oxygen, then add 50mL of N,N-dimethylformamide (DMF), keep at 120°C for 10h, after the reaction is complete, add 50mL of water, stir for 5 minutes, extract with 100mL×3 ethyl acetate, dry the organic phase, and use 95% ethanol Crystallization gave 7.4 g of yellow solid 2-methyl-1,2,3,9-tetrahydrobenzo[b]pyrrole[1,4]-thiazine-1,3-dione, yield 80.5%, mp: 237~239℃.