Preparation method of beta-glucose-based-Yariv reagent
A technology of glucosyl and glucoside, applied in the fields of chemical industry and medicine, can solve the problems of restricting the application and development of β-D-glucosyl-Yariv reagent, complicated operation, complicated process, etc., and achieves low production cost, low dosage, simple craftsmanship
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Embodiment 1
[0024] a, the preparation of p-aminophenylglucoside
[0025] Get the p-nitrophenyl glucoside 0.10g of 0.33mmol and add 10ml absolute methanol, mix and stir about 5 minutes, then add nickel content and be 0.30g of Raine nickel as metal catalyst of 10% (weight ratio), above-mentioned mixture and Put the Raney nickel catalyst together into the reactor, feed hydrogen with a pressure of 0.3MPa while continuously stirring, and perform a reduction reaction at 80°C for 3 hours. After the conversion is complete, cool to room temperature, filter through diatomaceous earth, and combine the filtrates Concentrate under reduced pressure to obtain p-aminophenyl glucoside, the pressure of the reduced-pressure concentration is 3.5KPa, the temperature is 30°C,
[0026] b, the preparation of diazonium salt
[0027] Dissolve the p-aminophenyl glucoside obtained by concentrating under reduced pressure in 2ml of pure water, then add 1ml of 0.5M hydrochloric acid and sodium nitrite solution dropwis...
Embodiment 2
[0031] a, the preparation of p-aminophenylglucoside
[0032] Get 3.3mmol of p-nitrophenyl glucoside 1.0g and add 90ml of absolute methanol, mix and stir for about 5 minutes, then add 0.20g of palladium catalyst with a palladium content of 10% (weight ratio), put the above mixture and palladium catalyst together into the reactor, feed hydrogen with a pressure of 0.5 MPa while continuously stirring, and perform a reduction reaction at 70°C for 4 hours. After the conversion is complete, cool to room temperature, filter through diatomaceous earth, combine the filtrates and concentrate under reduced pressure to obtain the right For aminophenyl glucoside, the pressure of vacuum concentration is 3.8KPa, and the temperature is 35°C.
[0033] b, the preparation of diazonium salt
[0034] Dissolve the p-aminophenyl glucoside obtained by the above-mentioned concentration under reduced pressure in 2ml of pure water, then add 10ml of 0.5M hydrochloric acid and sodium nitrite solution drop...
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