Category: 6299-25-8

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. 6299-25-8, name is 4,6-Dichloro-2-(methylthio)pyrimidine. A new synthetic method of this compound is introduced below., category: pyrimidines

Example 1 4,6-Dichloro-2-methanesulfonyl-pyrimidine A solution of 4,6-dichloro-2-(methylthio)pyrimidine (48.3 g, 247 mmol) in dichloromethane (1 L) was cooled on an ice bath. 3-Chloroperoxybenzoic acid (152 g, 619 mmol) was added portion-wise keeping the temperature below 10 C. The solution was allowed to warm to room-temperature and stirred over-night. The mixture was diluted with dichloromethane (2 L) and treated with an aqueous solution of sodium thiosulphate and sodium hydrogen carbonate (600 mL). The resulting mixture was stirred over-night. The phases were separated and the organic layer was washed with sodium hydrogencarbonate (500 mL) and brine (1 L), dried over sodium sulphate, filtrated and concentrated in vacuo. The resulting yellow solid was stirred with ether and 4,6-dichloro-2-methanesulfonyl-pyrimidine (32.6 g, 58%) was collected by filtration as a white solid.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine.

Reference:
Patent; NEUROSEARCH A/S; US2011/230484; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Reference of 6299-25-8, 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. 6299-25-8, name is 4,6-Dichloro-2-(methylthio)pyrimidine, molecular formula is C5H4Cl2N2S, 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.

Example 1 4,6-Dichloro-2-methanesulfonyl-pyrimidine A solution of 4,6-dichloro-2-(methylthio)pyrimidine (48.3 g, 247 mmol) in dichloromethane (1 L) was cooled on an ice bath. 3-Chloroperoxybenzoic acid (152 g, 619 mmol) was added portion-wise keeping the temperature below 10 C. The solution was allowed to warm to room-temperature and stirred over-night. The mixture was diluted with dichloromethane (2 L) and treated with an aqueous solution of sodium thiosulphate and sodium hydrogen carbonate (600 mL). The resulting mixture was stirred over-night. The phases were separated and the organic layer was washed with sodium hydrogencarbonate (500 mL) and brine (1 L), dried over sodium sulphate, filtrated and concentrated in vacuo. The resulting yellow solid was stirred with ether and 4,6-dichloro-2-methanesulfonyl-pyrimidine (32.6 g, 58%) was collected by filtration as a white solid.

According to the analysis of related databases, 6299-25-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NEUROSEARCH A/S; US2011/230484; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 6299-25-8, 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 6299-25-8, name is 4,6-Dichloro-2-(methylthio)pyrimidine. This compound has unique chemical properties. The synthetic route is as follows.

Commercially available 4,6-dichloro-2-methylthiopyrimidine (1.00 g, 5.13 mmol) was dissolved in THF (10 mL) and the mixture was stirred at -78C for 1 hour after adding a 2 anol/L lithium diisopropylamide/THF-ethylbenzene solution (5.9 mL, 11.8 mmol) at -78C. The mixture was then stirred for 1.5 hours at room temperature after adding dry ice at -78C. Thereafter, 10% hydrochloric acid and ethyl acetate were added to separate the organic layer. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was reslurried with hexane, and the resulting solid was filtered off to give 4,6-diohloro-2-methylthiopyrimidine-5-oarboxylic acid (964 mg, 79%). ESI-MS: m/z 237 [M – H]-. 1H-NMR (CDCl3) delta(ppm): 2.60 (s, 3H), 9.68 (brs, 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 6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine.

Reference:
Patent; Kyowa Hakko Kirin Co., Ltd.; EP2163554; (2010); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Adding a certain compound to certain chemical reactions, such as: 6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine, 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, Safety of 4,6-Dichloro-2-(methylthio)pyrimidine, blongs to pyrimidines compound. Safety of 4,6-Dichloro-2-(methylthio)pyrimidine

Commercially available 4,6-dichloro-2-methylthiopyrimidine (1.00 g, 5.13 mmol) was dissolved in THF (10 mL) and the mixture was stirred at -78C for 1 hour after adding a 2 anol/L lithium diisopropylamide/THF-ethylbenzene solution (5.9 mL, 11.8 mmol) at -78C. The mixture was then stirred for 1.5 hours at room temperature after adding dry ice at -78C. Thereafter, 10% hydrochloric acid and ethyl acetate were added to separate the organic layer. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was reslurried with hexane, and the resulting solid was filtered off to give 4,6-diohloro-2-methylthiopyrimidine-5-oarboxylic acid (964 mg, 79%). ESI-MS: m/z 237 [M – H]-. 1H-NMR (CDCl3) delta(ppm): 2.60 (s, 3H), 9.68 (brs, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine, and friends who are interested can also refer to it.

Reference:
Patent; Kyowa Hakko Kirin Co., Ltd.; EP2163554; (2010); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Adding a certain compound to certain chemical reactions, such as: 6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine, 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, Safety of 4,6-Dichloro-2-(methylthio)pyrimidine, blongs to pyrimidines compound. Safety of 4,6-Dichloro-2-(methylthio)pyrimidine

Commercially available 4,6-dichloro-2-methylthiopyrimidine (1.00 g, 5.13 mmol) was dissolved in THF (10 mL) and the mixture was stirred at -78C for 1 hour after adding a 2 anol/L lithium diisopropylamide/THF-ethylbenzene solution (5.9 mL, 11.8 mmol) at -78C. The mixture was then stirred for 1.5 hours at room temperature after adding dry ice at -78C. Thereafter, 10% hydrochloric acid and ethyl acetate were added to separate the organic layer. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was reslurried with hexane, and the resulting solid was filtered off to give 4,6-diohloro-2-methylthiopyrimidine-5-oarboxylic acid (964 mg, 79%). ESI-MS: m/z 237 [M – H]-. 1H-NMR (CDCl3) delta(ppm): 2.60 (s, 3H), 9.68 (brs, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine, and friends who are interested can also refer to it.

Reference:
Patent; Kyowa Hakko Kirin Co., Ltd.; EP2163554; (2010); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Reference of 6299-25-8 , The common heterocyclic compound, 6299-25-8, name is 4,6-Dichloro-2-(methylthio)pyrimidine, molecular formula is C5H4Cl2N2S, 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.

To a stirred solution of 4,6-dichloro-2- (methylthio)pyrimidine (50 g, 0.26 mol) in dichloromethane (1 L) at 00C was added meta-chloroperoxybenzoic acid (143.6 g, 0.64 mol) over a period of 20 minutes. The solution was allowed to warm to room temperature and was stirred for 4 hours. The mixture was diluted with dichloromethane (1.5 L) and then treated sequentially with 50% Na2S2O3 / NaHCO3 solution (2 x 200 ml), sat. NaHCO3 solution (4 x 300 ml), and brine (200 ml) then dried (MgSO4). The solvent was removed in vacuo to afford an off-white solid, which was redissolved in EtOAc (IL) and treated sequentially with sat. NaHCO3 solution (3 x 300 ml), and brine (100 ml) then dried (MgSO4). The solvent was removed EPO in vacuo to afford the title compound (A) as a white solid (55.6 g, 96% yield). 1H NMR CDCl3 delta 3.40 (3H5 s, CH3), 7.75 (IH. s. ArH).

The synthetic route of 6299-25-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; WO2007/14250; (2007); A2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Related Products of 6299-25-8 ,Some common heterocyclic compound, 6299-25-8, molecular formula is C5H4Cl2N2S, 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.

A mixture of 4,6-dichloro-2-(methylsulfanyl)pyrimidine (1-180) (20.0 g, 102.53 mmol) and oxone (189.0 g, 308 mmol) in THF (450 mL) and H20 (150 mL) was stirred at room temperature for 16 hr. TLC (Petroluem ether : EtOAc = 1 : 1) showed the starting material had been consumed. The reaction mixture was filtered and washed with THF (100 mL). The combined filtrate was concentrated, dissolved in EtOAc (500 mL) and washed with H20 (2 x 300 mL) and brine (300 mL). The organic layer was dried over Na2S04 and concentrated. The residue was purified by silica gel chromatography (petroleum ether : EtOAc = 10 : 1 to pure EtOAc) to give 4,6-dichloro- 2-(methylsulfonyl)pyrimidine (1-174) (20 g, 86 %) as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,6299-25-8, its application will become more common.

Reference:
Patent; PFIZER INC.; JOHNSON, Ted William; RICHARDSON, Paul Francis; COLLINS, Michael Raymond; RICHTER, Daniel Tyler; BURKE, Benjamin Joseph; GAJIWALA, Ketan; NINKOVIC, Sacha; LINTON, Maria Angelica; LE, Phuong Thi Quy; HOFFMAN, Jacqui Elizabeth; (335 pag.)WO2016/97918; (2016); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

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. 6299-25-8, name is 4,6-Dichloro-2-(methylthio)pyrimidine, the common compound, a new synthetic route is introduced below. Computed Properties of C5H4Cl2N2S

Prepared by methods substantially similar to those set forth in Koppell et al, JOC, 26,1961, 792, in the following manner. To a stirred solution of 4, 6-dichloro-2- (methylthio) pyrimidine (50 g, 0.26 mol) in dichloromethane [(1] L) at [0C] was added meta-chloroperoxybenzoic acid (143.6 g, 0.64 mol) over a period of 20 minutes. The solution was allowed to warm to room temperature and was stirred for 4 hours. The mixture was diluted with dichloromethane (1.5 L) and then treated sequentially with 50% [NA2S203/NAHC03] solution (2 x 200 ml), sat. [NAHC03] solution (4 x 300 ml), and brine (200 ml) then dried [(MGS04).] The solvent was removed in vacuo to afford an off-white solid which was redissolved in EtOAc [(1 L)] and treated sequentially with sat. [NAHC03] solution (3 x [300] ml), and brine (100 [ML)] then dried (MgS04). The solvent was removed in vacuo to afford the title compound (A) as a white solid (55.6 g, 96% yields NMR [CDC13] [5] 3.40 (3H, s, CH3), 7.75 [(1H.] s. ArH).

The synthetic route of 6299-25-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; WO2004/833; (2003); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Related Products of 6299-25-8, 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 6299-25-8 as follows.

LDA (2M in THF/n-heptane/ethylbenzene) (3.72 ml_, 28.2 mmol) was added dropwise to a solution of commercially available 4,6-dichloro-2-methylsulfanyl-pyrimidine (5 g, 25.63 mmol) in anhydrous THF (30 ml_) at -78 C under a nitrogen atmosphere and the mixture stirred for 1 hour. Ethyl chloroformate (2.7 ml_, 28.24 mmol) was added via syringe and the mixture stirred at -78 C for a further 2 hours and then allowed to warm to room temperature. The reaction was quenched by addition of saturated aqueous ammonium chloride solution (50 ml_) and extracted with EtOAc (2 x 50 ml_). The combined organic portions were dried over MgSCU and the solvent removed in vacuo. Purification by column chromatography on silica eluting with a gradient of 1 to 2% EtOAc in petrol afforded the titled compound as a yellow solid. (1376) LC-MS (Method 3B): Rt 2.52 mins; MS m/z N/A [does not ionise] (1377) 1 H NMR (500 MHz, Chloroform-d) d 4.45 (q, J = 7.1 Hz, 2H), 2.58 (s, 3H), 1.41 (t, J = 7.1 Hz, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,6299-25-8, its application will become more common.

Reference:
Patent; ADORX THERAPEUTICS LIMITED; MCCARTHY, Clive; MACLEOD, Calum; MOULTON, Ben; LENAGH-SNOW, Gabriel; (190 pag.)WO2019/122932; (2019); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Reference of 6299-25-8, 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. 6299-25-8, name is 4,6-Dichloro-2-(methylthio)pyrimidine, molecular formula is C5H4Cl2N2S, 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.

[00230] Reagents[00231] Experimental procedure:? ; Take ammonia in THF into a 2 L autoclave and add 4, 6-dichloro-2-(Methylthio) pyrimidine slowly.? Heat the reaction mixture to 50-60 C and maintain the reaction at 50-60 C for 3-4 hours (Inbuilt pressure 7- 8 Kg/cm ).? Check the progress of the reaction by TLC. Upon completion, the reaction was brought to 25-35 C.? Concentrate the reaction mixture under vacuum.? Charge Hexane and stir for 30-45 minutes at 25-35 C.? Filter the solid and wash the solid with Hexane.? Wash the solid with water (2X400 mL).? Dry the solid at 25-35 C till M.C reaches to less than 2%.Yield 352.0 g% of Yield: 97.77%.Purity by HPLC: 99.07%.Other suitable conditions such as ammonia in MeOH or dioxane could be used accordingly when different analogs are used. Example 1- 2. Preparation of 4-Amino-6-chloro-2- meth lthio)pyrimidine, 6.1

According to the analysis of related databases, 6299-25-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; KINAGEN, INC.; MURPHY, Eric, A.; CHERESH, David, A.; ARNORD, Lee, Daniel; WO2011/97594; (2011); A2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia