Chemical synthesis method for 2-formylcyanoacetylhydrazone-quinoxaline-1,4-dioxide
A formyl cyanoacetyl hydrazone and dioxide technology, which is applied in the field of pharmaceutical synthesis, can solve the problems of high cost, unreasonable synthetic intermediate route, inability to implement industrialized production, etc., and achieves low production cost, cheap raw materials, and low product high yield effect
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Embodiment 1
[0034] In a 4L four-neck flask, put 40.6g of benzofurazan and 60mL of acetone, and stir to dissolve them completely to obtain a dark red solution. Slowly add 1.5ml of tetrahydropyrrole (diluted with 10mL of acetone) dropwise with a dropping funnel at 45°C, the dropwise addition is completed within about 30min, and stirred for 2 hours. After the reaction, a large amount of light yellow solid precipitated out, cooled, filtered with suction, washed the product, dried at 70°C, and the yield was 61.5%.
[0035] In a 4L four-neck flask, add 100 mL of dimethyl sulfoxide and 5 mL of absolute ethanol, heat to 50°C, add 0.15 mol of selenium dioxide, stir to dissolve it completely, then add 0.1 mol of the above-mentioned solid, and continue the reaction for 5 hours. Leave overnight at room temperature. The reddish-brown solution was obtained by suction filtration, and the mixture was directly used in the next reaction.
[0036] Add 50 mL of absolute ethanol to the above filtrate, and a...
Embodiment 2
[0038] In a 4L four-neck flask, put 40.6g of benzofurazan and 75mL of acetone, stir to dissolve them completely, and obtain a dark red solution. At 60°C, 1.75ml of tetrahydropyrrole (diluted with 10mL of acetone) was slowly added dropwise with a dropping funnel, and the addition was completed within about 30 minutes, and stirred for 2 hours. After the reaction, a large amount of light yellow solid precipitated, cooled, filtered with suction, washed the product, dried at 70°C, and the yield was 62.3%.
[0039] In a 4L four-neck flask, add 100 mL of dimethyl sulfoxide and 10 mL of absolute ethanol, heat to 65°C, add 0.4 mol of selenium dioxide, stir to dissolve it completely, then add 0.2 mol of the above-mentioned solid, and continue the reaction for 7 hours. Leave overnight at room temperature. The reddish-brown solution was obtained by suction filtration, and the mixture was directly used in the next reaction.
[0040] In the above reaction filtrate, 50 mL of absolute ethan...
Embodiment 3
[0042] In a 4L four-neck flask, put 40.6g of benzofurazan and 90mL of acetone, stir to dissolve them completely, and obtain a dark red solution. Slowly add 2.0ml of tetrahydropyrrole (diluted with 10mL of acetone) dropwise with a dropping funnel at 75°C, the dropwise addition is completed within about 30min, and the stirring is continued for 2 hours. After the reaction, a large amount of light yellow solid precipitated, cooled, filtered with suction, washed the product, dried at 70°C, and the yield was 62.0%.
[0043] In a 4L four-neck flask, add 100 mL of dimethyl sulfoxide and 15 mL of absolute ethanol, heat to 85°C, add 0.6 mol of selenium dioxide, stir to dissolve it completely, then add 0.3 mol of the solid obtained above, and continue the reaction for 9 hours. Leave overnight at room temperature. After suction filtration, a reddish-brown solution was obtained, and the mixture was directly used in the next reaction.
[0044]In the above reaction filtrate, 80 mL of absol...
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