Category: 626-17-5

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 626-17-5, name is 1,3-Dicyanobenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H4N2

EXAMPLE 1 Hydrogenation of Isophthalonitrile Into a 100-ml autoclave, were charged 3.2 g of isophthalonitrile, 10.4 g of mesitylene, 10.0 g of liquid ammonia and 2.0 g of Pd-alumina pellets (manufactured by N.E. Chemcat Corporation; Pd content = 5% by weight), and the inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 95.7 mol%, the yield of 3-cyanobenzylamine was 87.3 mol% and the yield of m-xylynenediamine was 7.7 mol%. The reaction solution separated from the catalyst was charged into a 100-ml autoclave together with 10.0 g of liquid ammonia and 2.0 g of Ni-diatomaceous earth pellets (manufactured by Nikki Chemical Co., Ltd.; Ni supported amount = 46% by weight). The inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 100 mol%, the yield of 3-cyanobenzylamine was 0.2 mol% and the yield of m-xylynenediamine was 89.4 mol% EXAMPLE 4 Hydrogenation of Isophthalonitrile Into a 100-ml autoclave, were charged 3.2 g of isophthalonitrile, 10.4 g of mesitylene, 10.0 g of liquid ammonia and 2.0 g of Pd-alumina pellets (manufactured by N.E. Chemcat Corporation; Pd content = 5% by weight), and the inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 95.7 mol%, the yield of 3-cyanobenzylamine was 87.3 mol% and the yield of m-xylynenediamine was 7.7 mol%. The reaction solution separated from the catalyst was charged into a 100-ml autoclave together with 10.0 g of liquid ammonia and 2.0 g of the catalyst A. The inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 100 mol%, the yield of 3-cyanobenzylamine was 0.0 mol% and the yield of m-xylynenediamine was 91.1 mol%.

The synthetic route of 626-17-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MITSUBISHI GAS CHEMICAL COMPANY, INC.; EP1449825; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Synthetic Route of 626-17-5, A common heterocyclic compound, 626-17-5, name is 1,3-Dicyanobenzene, molecular formula is C8H4N2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 40 Isophthalonitrile (12.8 g), hydrogen chloride gas (2.24 NL), and methanol (72.5 g) were placed in a glass autoclave, and the mixture was allowed to react at 130 C. for seven hours. The reaction mixture was cooled, and water (9 g) was added thereto. Gas chromatographic analysis revealed that methyl m-cyanobenzoate had been produced at a yield of 38% and a selectivity of 83%.

The synthetic route of 626-17-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Showa Denko Kabushiki Kaisha; US6433211; (2002); B1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 626-17-5, name is 1,3-Dicyanobenzene, A new synthetic method of this compound is introduced below., Product Details of 626-17-5

EXAMPLE 1 Hydrogenation of Isophthalonitrile Into a 100-ml autoclave, were charged 3.2 g of isophthalonitrile, 10.4 g of mesitylene, 10.0 g of liquid ammonia and 2.0 g of Pd-alumina pellets (manufactured by N.E. Chemcat Corporation; Pd content = 5% by weight), and the inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 95.7 mol%, the yield of 3-cyanobenzylamine was 87.3 mol% and the yield of m-xylynenediamine was 7.7 mol%. The reaction solution separated from the catalyst was charged into a 100-ml autoclave together with 10.0 g of liquid ammonia and 2.0 g of Ni-diatomaceous earth pellets (manufactured by Nikki Chemical Co., Ltd.; Ni supported amount = 46% by weight). The inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 100 mol%, the yield of 3-cyanobenzylamine was 0.2 mol% and the yield of m-xylynenediamine was 89.4 mol% EXAMPLE 4 Hydrogenation of Isophthalonitrile Into a 100-ml autoclave, were charged 3.2 g of isophthalonitrile, 10.4 g of mesitylene, 10.0 g of liquid ammonia and 2.0 g of Pd-alumina pellets (manufactured by N.E. Chemcat Corporation; Pd content = 5% by weight), and the inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 95.7 mol%, the yield of 3-cyanobenzylamine was 87.3 mol% and the yield of m-xylynenediamine was 7.7 mol%. The reaction solution separated from the catalyst was charged into a 100-ml autoclave together with 10.0 g of liquid ammonia and 2.0 g of the catalyst A. The inner pressure was raised to 4.9 MPa by hydrogen gas. Then, the autoclave was shaken at 50C until the change of pressure was no longer appreciated. The analysis on the reaction product solution showed that the conversion of isophthalonitrile was 100 mol%, the yield of 3-cyanobenzylamine was 0.0 mol% and the yield of m-xylynenediamine was 91.1 mol%.

The synthetic route of 626-17-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MITSUBISHI GAS CHEMICAL COMPANY, INC.; EP1449825; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Reference of 626-17-5, These common heterocyclic compound, 626-17-5, name is 1,3-Dicyanobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The same type of sponge nickel catalyst as used in Comparative Example 5 was charged into a glass tube with a 10-mm inner diameter in an amount of 3 g and dried at 200 C. in a nitrogen stream. Then, a mixed gas (methanol:nitrogen=4:96 by volume) was allowed to pass through the catalyst bed to pretreat the catalyst under the conditions of atmospheric pressure, 200 C., a flow rate of 1.5 NL/h, and 3 h. After the pretreatment, the catalyst was cooled to 30 C. in a nitrogen gas flow. The pretreated catalyst was slurried in 60 g of methanol in a nitrogen atmosphere. The hydrogenation of isophthalonitrile was conducted in the same manner as in Comparative Example 5 except for using the pretreated catalyst thus prepared. After 4 h of the hydrogenation, a part of the reaction liquid was sampled and analyzed. The conversion of isophthalonitrile was 100 mol %, the yield of m-xylylenediamine was 92.8 mol %, the yield of 3-cyanobenzylamine was 0.2 mol %, and the yield of high-boiling condensation products was 7 mol %.

The synthetic route of 626-17-5 has been constantly updated, and we look forward to future research findings.

626-17-5, Name is 1,3-Dicyanobenzene, 626-17-5, belongs to nitriles-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows.

EXAMPLE 11; The hydrogenation was conducted in the same manner as in Example 2 except for changing the starting solution to a mixture of 1 part by weight of the starting isophthalonitrile, 8 parts by weight of liquid ammonia and 1 part by weight of m-xylene. The first hydrogenation product solution discharged from the reaction tube A was sampled just before entering into the reaction tube B and analyzed by a gas chromatography. The conversion of the starting isophthalonitrile was 95.4 mol %, the selectivity of m-xylylenediamine was 84.5 mol %, and the selectivity of 3-cyanobenzylamine was 6.20 mol %. In addition, 83.6% of the total nitrile groups in the starting isophthalonitrile were hydrogenated to aminomethyl groups in the hydrogenation step 1. The second hydrogenation product solution and unreacted hydrogen gas were discharged from the outlet of the reaction tube B. The discharged second hydrogenation product solution was sampled and analyzed by a gas chromatography. The amount of 3-cyanobenzylamine was 0.057% by weight on the basis of the weight of m-xylylenediamine. The conversion of isophthalonitrile was 99.9 mol % or more, the selectivity of m-xylylenediamine was 90.6 mol % and the selectivity of 3-cyanobenzylamine was 0.0530 mol %, each being the overall value throughout the hydrogenation step 1 and the hydrogenation step 2. After evaporating off ammonia from the second hydrogenation product solution, the crude m-xylylenediamine was distilled under reduced pressure (125 C., 6 Torr). The purified product contained 99.94% by weight of m-xylylenediamine and 580 ppm by weight of 3-cyanobenzylamine when determined by a gas chromatography.

Statistics shows that 1,3-Dicyanobenzene is playing an increasingly important role. we look forward to future research findings about 626-17-5.

Reference:
Patent; Kumano, Tatsuyuki; Shigematsu, Ryusuke; Kato, Kinji; Nakaya, Kenji; US2008/9654; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts