1-METHYL-1,3-DIHYDRO-BENZO[1,2,5]THIADIAZOLE 2,2-DIOXIDE synthesis
- Product Name:1-METHYL-1,3-DIHYDRO-BENZO[1,2,5]THIADIAZOLE 2,2-DIOXIDE
- CAS Number:443987-59-5
- Molecular formula:C7H8N2O2S
- Molecular Weight:184.22
4760-34-3
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Yield:443987-59-5 56%
Reaction Conditions:
with pyridine;SULFAMIDE at 120; for 1 h;Inert atmosphere;
Steps:
110.3 3. Synthesis of intermediate 110-3
3. Synthesis of intermediate 110-3 Under a nitrogen atmosphere, the intermediate 110-2 (10.0 g, 81.9 mmol) as a raw material was dissolved in 500 mL of pyridine in a 1000 mL three-necked flask at room temperature and sulfonamide (7.8 g, 81.2 mmol) was added to the reaction flask. After completion of the reaction, the reaction was heated to 120°C and carried out for 1 hour. After detecting the reaction was completed, the reaction system was cooled to room temperature. The reaction mixture was concentrated to dryness. The resulting residue was purified by silica gel column chromatography (eluent: PE: EA = 10: 1-1: 1), and then the resulting product was collected and concentrated to dryness to give 8.5 g of the intermediate 110-3 (56%) as a brown solid. LCMS: 185.0.
References:
EP3216786,2017,A1 Location in patent:Paragraph 0573-0574
1493-27-2
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612-28-2
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