Method of synthesizing 1-methyl hydantoin
A synthesis method, the technology of methylhydantoin, applied in the field of synthesis of 1-methylhydantoin, can solve the problems of complicated synthetic routes and the use of highly toxic drugs, and achieve improved safety, reduced synthetic costs, and simple and easy synthetic routes line effect
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Embodiment 1
[0009] Add 46.5 g of 30% methylamine aqueous solution, 106 g of 10% sodium carbonate aqueous solution, and 87.5 g of 20% sodium chloroacetate aqueous solution into a 500 ml four-necked bottle, and react at 50° C. for 4 hours. Methylamine was distilled off and the pH was adjusted to 2. Heat to 100°C, add 91g of 8% sodium cyanate aqueous solution dropwise under reflux, stir and react for 30 minutes, add 7.3g of solid sodium cyanate to continue the reaction for 90 minutes, cool to 5°C, add 25g of 98% concentrated sulfuric acid , heated to 100° C. for reflux reaction for 2 hr, and evaporated to dryness under reduced pressure to obtain 9.85 g (59.4%) of crude product. The synthesized product is recrystallized and purified with chloroform, and the purity of the purified product can reach more than 99% through high performance liquid phase detection.
Embodiment 2
[0011] Add 46.5 g of 30% methylamine aqueous solution, 106 g of 10% sodium carbonate aqueous solution, and 87.5 g of 20% sodium chloroacetate aqueous solution into a 500 ml four-necked bottle, and react at 60° C. for 4 hours. Methylamine was distilled off and the pH was adjusted to 2. Heat to 100°C, add 91g of 8% sodium cyanate aqueous solution dropwise under reflux, stir and react for 30 minutes, add 7.3g of solid sodium cyanate to continue the reaction for 90 minutes, cool to 5°C, add 25g of 98% concentrated sulfuric acid , heated to 100° C., refluxed for 2 hr, and evaporated to dryness under reduced pressure to obtain 10.77 g (62.5%) of crude product. The synthesized product is recrystallized and purified with chloroform, and the purity of the purified product can reach more than 99% through high performance liquid phase detection.
Embodiment 3
[0013] Add 46.5 g of 30% methylamine aqueous solution, 106 g of 10% sodium carbonate aqueous solution, and 87.5 g of 20% sodium chloroacetate aqueous solution into a 500 ml four-necked bottle, and react at 70° C. for 4 hours. Methylamine was distilled off and the pH was adjusted to 2. Heat to 100°C, add 91g of 8% sodium cyanate aqueous solution dropwise under reflux, stir and react for 30 minutes, add 7.3g of solid sodium cyanate to continue the reaction for 90 minutes, cool to 5°C, add 25g of 98% concentrated sulfuric acid , heated to 100° C., refluxed for 2 hr, and evaporated to dryness under reduced pressure to obtain 10.18 g (61.4%) of crude product. The synthesized product is recrystallized and purified with chloroform, and the purity of the purified product can reach more than 99% through high performance liquid phase detection.
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