Month: April 2022

Reference of 1235036-15-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1235036-15-3, name is tert-Butyl 3-bromo-6-chloropicolinate, molecular formula is C10H11BrClNO2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a solution of tert-butyl 3-bromo-6-chloropicolinate (3.06 g) in tetrahydrofuran (50 mL)and water (20 mL) was added Example 1.14.1 (4.45 g), 1,3,5,7-tetramethyl-8-tetradecyl-2,4,6-trioxa-8-phosphaadamantane (0.732 g), Pd2(dba)3 (0.479 g), and K3P04 (11 g). The mixture was stirred atreflux overnight and concentrated. The residue was dissolved in ethyl acetate (500 mL) and washedwith water and brine. The organic layer was dried over Na2S04, filtered, and concentrated. The residue was purified by flash chromatography, eluting with a gradient of 20-40% ethyl acetate indichloromethane, to provide the title compound. MS (ESI) m/e 530.23 (M+Ht.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1235036-15-3, tert-Butyl 3-bromo-6-chloropicolinate.

Reference:
Patent; ABBVIE INC.; BOGHAERT, Erwin, R.; JUDD, Andrew, S.; PHILLIPS, Andrew, C.; SOUERS, Andrew, J.; BRUNCKO, Milan; (503 pag.)WO2017/214301; (2017); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 107867-51-6, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 107867-51-6, name is 5-(Trifluoromethyl)pyridine-2,3-diamine, molecular formula is C6H6F3N3, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a mixed solution of 300 mg of 1- [3- (ethylsulfonyl) -6-iodoimidazo [1,2-a] pyridin-2-yl] ethan-1-one and 5 ml of dimethylsulfoxide was added 48 mass% 1 ml of hydrochloric acid was added.After completion of the addition, the reaction mixture was stirred at 80 C. for 2 hours. After completion of the stirring, 141 mg of 5- (trifluoromethyl) pyridine-2,3-diamine was added to the reaction mixture at room temperature.After the addition was completed, the reaction mixture was stirred at room temperature for 16 hours. After completion of the reaction, 10 ml of water was added to the reaction mixture at room temperature. After completion of the addition, sodium hydrogencarbonate was added to the reaction mixture for neutralization, followed by extraction with ethyl acetate (20 ml × 2).The obtained organic layer was dehydrated with anhydrous sodium sulfate and dried, and then the solvent was distilled off under reduced pressure. The precipitated solid was filtered off by filtration.The resulting solid was washed with diisopropyl ether to give the desired product 3- [3- (ethylsulfonyl) -6-iodoimidazo [1,2-a] pyridin-2-yl] – 7 – (trifluoromethyl ) Pyrido [2,3-b] pyrazine as a yellow solid.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 107867-51-6, 5-(Trifluoromethyl)pyridine-2,3-diamine.

Reference:
Patent; CD: Nissan Chemical Industries, Inc.; Noto Kenkichi; Kudo Takao; Matsui Yo Jin; Kobayashi Masaki; (50 pag.)JP2018/27943; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 184416-84-0, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 184416-84-0 as follows.

A solution of sodium hydride (60% in mineral oil, 600 mg, 15.0 mmol, 3 equiv.) in hexanol (10 ml) was stirred at r.t. for 2 h. 2,3-Dichloro-isonicotinic acid (960 mg, 5.0 mmol, 1 equiv.) was added and the reaction mixture was stirred at 1000C for 16 h. The mixture was diluted with water (100 ml) and pentane (300 ml), and the two phases were separated. The aqueous phase was neutralised with 1N HCI solution to pH 6.0 and extracted with EtOAc (3×80 ml). The combined EtOAc extracts were dried (MgSO4) and evaporated under reduced pressure to dryness. The residue was triturated with pentane, cooled at 00C and the precipitant solid was filtered, to give 410 mg of a white compound (yield 32%). By 1H-NMR analysis, it consisted of about 80% of the desired product, which was used to the next step without further purification. HPLC-MS: m/z 256 [M-H]”, Rt = 2.94 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,184416-84-0, its application will become more common.

Reference:
Patent; PROLYSIS LTD; WO2007/107758; (2007); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 18699-87-1, name is 2-Methyl-3-nitropyridine, the common compound, a new synthetic route is introduced below. Recommanded Product: 18699-87-1

Step 2: 2-bromomethyl-3-nitropyridine; 2,2′-azobis(isobutyronitrile) (2.7 g, 16.4 mmol) was added to a solution of2-methyl-3-nitropyridine (12.97 g, 92.6 mmol) prepared in Step 1 and N- bromo-succinimide (23.06 g, 130 mmol) in carbon tetrachloride (100 ml) and then the reactionmixtue was refluxed for 3 days. The reaction mixture was cooled to room temperatureand then concentrated under reduced pressure. The resulting residue was diluted withethyl acetate (100 ml) and then washed with a saturated sodium bicarbonate solutionand a saturated sodium thiosulfate solution. The organic layer was dried on anhydrousmagnesium sulfate and then purified with silica gel column chromatography(dichloromethane/n-hexane=2/l, v/v) to give 7.5 g of the titled compound as brown oil. lH-NMR(400MHz, CDC1) 5 8.82(d, 1H), 8.39(d, 1H), 7.56(t, 1H), 5.07(s, 2H)

The synthetic route of 18699-87-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; YUHAN CORPORATION; JANG, Sun-Young; WO2006/25716; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 1256785-40-6, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 1256785-40-6, name is Methyl 4-amino-6-chloronicotinate. This compound has unique chemical properties. The synthetic route is as follows.

Step 1: Methyl 4-amino-6-chloronicotinate (15 g, 80 mmol) obtained by the method described in US2012/184562 and sodium hydroxide (13 g, 322 mmol) were stirred in a mixed solution of methanol (100 mL) and water (50 mL) at room temperature for 12 hours. The reaction mixture was adjusted to pH 6 with a 6.0 mol/L aqueous hydrochloric acid solution, and the resulting solid was collected by filtration, whereby 4-amino-6-chloronicotinic acid (8.0 g, yield: 58%) was obtained. 1H-NMR (300 MHz, DMSO-d6, delta): 8.47 (s, 1H), 7.52 (br s, 2H), 6.75 (s, 1H)

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1256785-40-6, Methyl 4-amino-6-chloronicotinate.

Reference:
Patent; KYOWA HAKKO KIRIN CO., LTD.; ISHIDA, Hiroshi; MOTOSAWA, Keiichi; MIURA, Yusuke; NAKAI, Ryuichiro; OKADA, Ryoko; TAKAHASHI, Yuichi; (45 pag.)US2016/168125; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 53636-70-7, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 53636-70-7 as follows.

In a 100 ml round-bottomed flask 6-methyl-2,3-pyridinedicarboxylic acid (10 g, 55.2 mmol) and acetic anhydride (26 ml, 276 mmol) were added and heated at 100 0C under nitrogen for 5 hours. After this time the volatiles were removed under vacuum to give the title compound D32 (8.2 g) as a slightly brown solid. 1H NMR (400 MHz, DMSO-J6) delta ppm 8.41 (d, 1 H), 7.82 (d, 1 H), 2.73 (s, 3 H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,53636-70-7, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; ALVARO, Giuseppe; AMANTINI, David; CASTIGLIONI, Emiliano; DI FABIO, Romano; PAVONE, Francesca; WO2010/63662; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 106014-21-5, 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. 106014-21-5, name is Dimethyl 3-chloropyridine-2,5-dicarboxylate. A new synthetic method of this compound is introduced below.

To a solution of dimethyl 3-chloropyridine-2,5-dicarboxylate (1.0 g, 4.4 mmol) in THF(10 mL) and MeOH (20 mL) was added powdered calcium chloride (3.9 g, 35 mmol). The suspension was cooled to 00C and sodium borohydride (416 mg, 11.0 mmol) was added portionwise. The resulting mixture was stirred for 3 h at 00C and poured into ice-water (200 mL), and extracted with DCM (2 x 100 mL). The combined organic layers were dried (Na2SO4), filtered and the solvent was removed in vacuo to yield methyl 5-chloro-6- (hydroxymethyl)nicotinate which was used in the next step without further purification. GC/MS (m/z): 201.0

At the same time, in my other blogs, there are other synthetic methods of this type of compound,106014-21-5, Dimethyl 3-chloropyridine-2,5-dicarboxylate, and friends who are interested can also refer to it.

Reference:
Patent; JERINI AG; WO2009/36996; (2009); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 4684-94-0, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.4684-94-0, name is 6-Chloropicolinic acid, molecular formula is C6H4ClNO2, molecular weight is 157.55, as common compound, the synthetic route is as follows.

To 500mL three-necked flask equipped with a thermometer, was added DMF (200ml), between sequentially added trifluoromethylphenol (0.26mol, 42.2g), potassium carbonate (0.266mol, 37.2g), 2-chloro-6-carboxy pyridine (0.2mol, 31.6g), cuprous chloride (1.0 g of), heated to 140 deg.] C, the reaction 6.0H, cooled to room temperature, the reaction solution was poured into 600ml of ice water, pH = 3 adjusted with concentrated brine, and the precipitated solid was pumped was filtered off, washed with water, dried to obtain a white solid, yield: 75%

The chemical industry reduces the impact on the environment during synthesis 4684-94-0, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Chen Lei; (6 pag.)CN108530351; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 69045-78-9, 2-Chloro-5-(trichloromethyl)pyridine, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Recommanded Product: 69045-78-9, blongs to pyridine-derivatives compound. Recommanded Product: 69045-78-9

Example 4 In a 3000 cc autoclave equipped with a magnetic stirrer, a 40% aqueous solution of methylamine (814 g), ethanol (312 g) and Raney nickel (35 g) were charged. Hydrogen gas was introduced into the autoclave to a pressure of 3 Kg/cm2. While keeping a temperature at 30 C. or lower and supplying the hydrogen gas, a 58.8% solution of 2-chloro-5-trichloromethylpyridine in toluene (589 g) was added over 40 minutes. After the addition of the solution of 2-chloro-5-trichloromethylpyridine, the internal temperature was gradually raised to 40 C. At the same temperature, the hydrogen gas was supplied till the absorption of hydrogen ceased. After completion of reaction, the autoclave was cooled to room temperature, and the catalyst was filtrated off from the reaction mixture. The filtrate was analyzed by high pressure liquid chromatography to find that a yield of 2-chloro-5-methylaminomethylpyridine was 76%.

The synthetic route of 69045-78-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Koei Chemical Co., Ltd.; US5424437; (1995); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.184416-84-0, name is 2,3-Dichloroisonicotinic acid, molecular formula is C6H3Cl2NO2, molecular weight is 192, as common compound, the synthetic route is as follows.Application In Synthesis of 2,3-Dichloroisonicotinic acid

A mixture of 2,3-dichloroisonicotinic acid (960 mg, 5.00 mmol) and BH3 FontWeight=”Bold” FontSize=”10″ THF (1.0 M, 25 mL, 25 eq) was heated at 60 C for 4 h. After cooling to RT, MeOH (5 mL) was added, and the volatiles were removed under reduced pressure. The reaction mixture was diluted with water (50 mL) and extracted with DCM (50 mL x 3). The combined organic phase was washed with brine (100 mL), dried over Na2SC>4, filtered and concentrated to give (2,3- dichloropyridin-4-yl)methanol (400 mg, 45%) as a white solid. MS (ES+) C6H5C12N0 requires: 178, found: 179 [M+H]+. XH NMR (500 MHz, i-DMSO) delta 8.38 (d, J = 5 Hz, 1H), 7.58 (d, J= 5 Hz, 1H), 5.85-5.75 (br s, 1 H), 4.61 (s, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,184416-84-0, 2,3-Dichloroisonicotinic acid, and friends who are interested can also refer to it.

Reference:
Patent; TESARO, INC.; JONES, Philip; CZAKO, Barbara; BURKE, Jason P.; CROSS, Jason; LEONARD, Paul Graham; TREMBLAY, Martin; MANDAL, Pijus; (232 pag.)WO2018/119387; (2018); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem