25229-97-4Relevant articles and documents
Preparation method for hemisulphate
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Paragraph 0039-0041; 0044-0046; 0049-0051, (2019/10/10)
The invention provides a preparation method for hemisulphate, and relates to the technical field of organic synthesis. The method comprises the following steps: step 1, dissolving malonamide nitrile, triethyl orthoformate and morpholine in absolute ethyl alcohol, raising the temperature for refluxing, and cooling to 15-25 DEG C after the reaction is completed; step 2, separating out solids from a mixture obtained in step 1, centrifuging, washing with ethyl alcohol, recrystallizing by using ethyl alcohol refluxing, cooling to 15-25 DEG C, then centrifuging, washing with ethyl alcohol, and drying to obtain a pre-product A; step 3, adding the pre-product A into water, heating to 50-80 DEG C, dropwise adding hydrazine hydrate, raising the temperature to 100-115 DEG C, reacting under refluxing for 25-35 min, and cooling to 15-25 DEG C to obtain a pre-product B; step 4, adjusting the pH of the pre-product B to be acid, cooling to 15-25 DEG C to separate out solids, centrifuging, washing, heating the solids to 75-85 DEG C with water, adding activated carbon and stirring for 10-15 min, filtering, centrifuging, washing, and drying to obtain a product. The method provided by the invention has the beneficial effects that the reaction temperature and time are quantitatively controlled, and the recovery rate of the final product of hemisulphate reaches 85% or above.
Synthetic method of 1H-pyrazolo[3,4-d]pyrimidine-4-ol
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Paragraph 0024-0026; 0031, (2018/11/27)
The invention discloses a synthetic method of 1H-pyrazolo[3,4-d]pyrimidine-4-ol. According to the method, triethyl orthoformate, morpholine and cyanoacetamide are used as basic raw materials, a solvent acetonitrile medium is replaced, 2-cyan-3-morpholine acrylamide is synthesized, the use of a traditional highly acid sulfuric acid raw material is abandoned, and organic acid is used as a catalyst to replace sulfuric acid. The original traditional three-step synthesis process is simplified to two-step process, and the synthesis route is shortened. Then, raw material cost is reduced, and the operation is simplified. By the synthetic method, product yield is increased, and generation of ''three wastes (waste gas, waste water and industrial residue) '' is reduced.
Reaction of Ortho Esters with Secondary Amines
Swaringen, Roy A.,Eaddy, John F.,Henderson, Thomas R.
, p. 3986 - 3989 (2007/10/02)
The scope of the reaction of ortho esters with secondary amines has been explored.With p-toluenesulfonic acid as catalyst, N-alkylanilines and orthoformates gave high yields of N-alkylformanilides and N,N-dialkylanilines in contrast to previous work with other acid catalysts where ortho amides were produced in low yield.Aliphatic cyclic amines (e.g., morpholine, piperidine) and orthoformates gave the corresponding ortho amides.This constitutes a new convenient synthesis of these useful reagents.
