A kind of carbamazepine antigen and preparation method thereof
A carbamazepine and antigen technology, which is applied in the field of carbamazepine antigen and its preparation, can solve the problems of being unsuitable for batch sample screening detection and on-site instant detection, expensive and other problems, and achieves high product yield, strong specificity, and preparation process. simple steps
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[0032] A preparation method for carbamazepine antigen, comprising the following steps:
[0033] (1) Synthesis of 10-methoxy-5H-dibenzo[b, f]azepine-5-carboxamide (II)
[0034]
[0035] Under nitrogen protection, dissolve 10-methoxy-5H-dibenzo(b,f)azepine (I) in dichloromethane, lower the temperature to 0-5°C, add chlorosulfonyl isocyanate, the The mass ratio of carbamazepine and chlorosulfonyl isocyanate is 1:0.8-1. After the addition, the temperature is raised to 20-30° C. for 12-18 hours. Add water, adjust the pH to 8-9 with 1N sodium hydroxide solution, add dichloromethane, extract and separate layers, wash the organic layer with water, dry the organic layer over anhydrous sodium sulfate, and concentrate under reduced pressure to obtain 10-methoxy-5H-diphenyl And [b, f] azepine-5-carboxamide (II).
[0036] (2) Synthesis of 10-hydroxyl-5H-dibenzo[b, f]azepine-5-carboxamide (III)
[0037]
[0038] Under nitrogen protection, dissolve 10-methoxy-5H-dibenzo[b,f]azepine-...
Embodiment 1
[0046] A preparation method for carbamazepine antigen, comprising the following steps:
[0047](1) Synthesis of 10-methoxy-5H-dibenzo[b, f]azepine-5-carboxamide (II)
[0048] Under nitrogen protection, dissolve 45mg of 10-methoxy-5H-dibenzo(b,f)azepine (I) in 10mL of dichloromethane, lower the temperature to 0-5°C, add 40mg of chlorosulfonyl isocyanate, After the addition, the temperature was raised to 25°C for 15 hours. Add 10 mL of water, adjust the pH to 8.2 with 1N sodium hydroxide solution, add 30 mL of dichloromethane, extract and separate layers, wash the organic layer with 10 mL of water, dry the organic layer over anhydrous sodium sulfate, and concentrate under reduced pressure to obtain 58 mg of 10-methoxy- 5H-Dibenzo[b,f]azepine-5-carboxamide (II).
[0049] (2) Synthesis of 10-hydroxyl-5H-dibenzo[b, f]azepine-5-carboxamide (III)
[0050] Under nitrogen protection, 58mg of 10-methoxy-5H-dibenzo[b,f]azepine-5-carboxamide (II) was dissolved in 30mL of dichloromethan...
Embodiment 2
[0056] A preparation method for carbamazepine antigen, comprising the following steps:
[0057] (1) Synthesis of 10-methoxy-5H-dibenzo[b, f]azepine-5-carboxamide (II)
[0058] Under nitrogen protection, dissolve 45mg of 10-methoxy-5H-dibenzo(b, f)azepine (I) in 12mL of dichloromethane, lower the temperature to 0-5°C, add 41mg of chlorosulfonyl isocyanate After the addition, the temperature was raised to 25°C for 16h. Add 10 mL of water, adjust the pH to 8.7 with 1N sodium hydroxide solution, add 40 mL of dichloromethane, extract and separate layers, wash the organic layer with 10 mL of water, dry the organic layer over anhydrous sodium sulfate, and concentrate under reduced pressure to obtain 59 mg of 10-methoxy- 5H-Dibenzo[b,f]azepine-5-carboxamide (II).
[0059] (2) Synthesis of 10-hydroxyl-5H-dibenzo[b, f]azepine-5-carboxamide (III)
[0060] Under nitrogen protection, dissolve 59mg of 10-methoxy-5H-dibenzo[b,f]azepine-5-carboxamide (II) in 30mL of dichloromethane, lower ...
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