Synthetic method of amifostine
A synthesis method and technology of amifostine, applied in the field of chemical medicine, can solve the problems of high equipment requirements, low yield and high cost, and achieve the effects of high purity, simple post-processing and ideal yield
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Embodiment 1
[0032] The synthesis of embodiment 1 amifostine
[0033] (1) compound (114g) shown in formula (Ⅳ) is added in the reactor, adds rhodium oxide 0.66g, gold oxide 1.30g and Raney nickel 2.6g, then intermittently feeds hydrogen from the bottom of the kettle, every time Enter the amount of hydrogen so that the pressure in the reactor is about 2 MPa, heat up to 82-83 ° C, react for 18 hours, cool down to room temperature after the reaction, and filter out rhodium oxide, gold oxide and Raney nickel to obtain formula (Ⅲ) Compound 115.9g, yield 98.2%, purity 99%;
[0034] (2) On the basis of the compound represented by the formula (III) prepared above, add 405 mL of ethanol, and dissolve the aqueous solution of hydrogen bromide (10% by mass, containing bromine) at 13-15 ° C within 2 hours Hydrogen 90g) was added to the compound shown in formula (III), continued to react for 1h, then rectified, evaporated to dryness under reduced pressure, added activated carbon and methanol to reflux ...
Embodiment 2
[0036] The synthesis of embodiment 2 amifostine
[0037] (1) compound (228g) shown in formula (Ⅳ) is added in the reactor, adds rhodium oxide 1.75g, gold oxide 4.38g and Raney nickel 5.27g, then intermittently feeds hydrogen from the bottom of the kettle, every time Enter the amount of hydrogen so that the pressure in the reactor is about 2 MPa, heat up to 82-83 ° C, react for 20 hours, cool down to room temperature after the reaction, and filter out rhodium oxide, gold oxide and Raney nickel to obtain formula (Ⅲ) Compound 231.3g, yield 98%, purity 99.2%;
[0038] (2) On the basis of the compound represented by the formula (III) prepared above, add 405 mL of ethanol, and dissolve the aqueous solution of hydrogen bromide (10% by mass, containing bromine) at 13-15 ° C within 2 hours Hydrogen 90g) was added to the compound shown in formula (III), continued to react for 1h, then rectified, evaporated to dryness under reduced pressure, added activated carbon and methanol to reflux...
Embodiment 3
[0040] The synthesis of embodiment 3 amifostine
[0041](1) Compound (114g) shown in formula (Ⅳ) is added in the reactor, adds rhodium oxide 0.70g, gold oxide 1.30g and Raney nickel 2.6g, then intermittently feeds hydrogen from the bottom of the kettle, every time Enter the amount of hydrogen so that the pressure in the reactor is about 1.5 MPa, heat up to 82-83 ° C, react for 15 hours, cool down to room temperature after the reaction, and suck out rhodium oxide, gold oxide and Raney nickel to obtain the formula (Ⅲ) Compound 115g was shown, the yield was 97.5%, and the purity was 99.5%;
[0042] (2) On the basis of the compound represented by the formula (III) prepared above, add 450 mL of ethanol, and dissolve an aqueous solution of hydrogen bromide (10% by mass, containing Add 100 g of hydrogen bromide to the compound shown in formula (III), continue to react for 1 h, then rectify, evaporate to dryness under reduced pressure, add activated carbon and methanol to reflux for ...
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