Month: February 2021

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 363-51-9, name is 2-Chloro-6-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H5ClFN

General procedure: NaOt-Bu (0.240 g, 2.5 mmol), Pd(OAc)2 (0.006 g, 0.025 mmol) and [HPt-Bu3][BF4] (0.010 g, 0.035 mmol) were suspended in toluene (3 ml) in a 5 ml microwave vial. The appropriate 2-chloroaniline (0.50 mmol) and aryl bromide (0.50 mmol) were then added and the vial sealed. The reaction was then heated in the microwave reactor at 160 C for 3 h, allowed to cool, and then quenched by addition of aqueous HCl (2 M, 3 ml). The organic phase was extracted with CH2Cl2 (2¡Á20 ml), dried (MgSO4), then filtered and the solvent removed under reduced pressure. The crude product mixture was then subjected to column chromatography (SiO2).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 363-51-9.

Reference:
Article; Bedford, Robin B.; Bowen, John G.; Weeks, Amanda L.; Tetrahedron; vol. 69; 22; (2013); p. 4389 – 4394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 139512-70-2,Some common heterocyclic compound, 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, molecular formula is C6H6ClFN2, 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.

General procedure: A mixture of compounds 1a-l (0.013 mol) and 4-chloro-5-fluoro-ophenylenediamine(2) (0.01 mol) in methanol (10 mL) was irradiatedwith ultrasonic irradiation at 50 C for 7 min (8 min for 3a) Afterreaction completion (monitored by TLC, ethyl acetate/hexane = 3:1), themixture was poured onto water and the precipitated product was filtrated off, washed with water and recrystallised from ethanol/water, 3:1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Chloro-5-fluorobenzene-1,2-diamine, its application will become more common.

Reference:
Article; Mente?e, Emre; Kahveci, Bahittin; Mente?e, Meltem; Journal of Chemical Research; vol. 42; 6; (2018); p. 329 – 331;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 172921-33-4, name is 1-Bromo-4-chloro-2,5-difluorobenzene, belongs to chlorides-buliding-blocks compound, 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 172921-33-4, Recommanded Product: 1-Bromo-4-chloro-2,5-difluorobenzene

1-Bromo-4-chloro-2,5-difluorobenzene (1.11 g, 4.9 mmol) was dissolved in tetrahydrofuran (THF; 15 mL) and cooled to -10¡ã C. A 2.0M solution of isopropyl-magnesium chloride (2.7 mL, 5.4 mmol) in THF was added dropwise via syringe. The reaction mixture was stirred at -10¡ã C. for 1 h, allowed to warm toward 0¡ã C. for 1 h, then cooled again to -10¡ã C. A solution of 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.0 g, 5.4 mmol) in THF (1.0 mL) was then added dropwise and the reaction mixture was allowed to warm to ambient temperature. The reaction mixture was then added to diethyl ether and extracted with 1N sodium hydroxide twice. The aqueous phases were combined, acidified to pH 3 with concentrated HCl, and extracted with dichloromethane twice. The organic phases were combined, dried, filtered and concentrated to give the title compound (0.97 g, 72.3percent yield) that was used without further purification: 1H NMR (CDCl3) delta 7.45 (dd, 1H), 7.09 dd, 1H), 1.36 (s, 12H).

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.

Reference:
Patent; Dow AgroSciences LLC; US2009/88322; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 6940-78-9, name is 1-Bromo-4-chlorobutane, A new synthetic method of this compound is introduced below., Quality Control of 1-Bromo-4-chlorobutane

Step 1: Synthesis of 1-(4-Chlorobutyl)-1,5,6,7-tetrahydroindol-4-one To a solution of 1,5,6,7-tetrahydroindol-4-one (10.0 g) in DMSO (100 mL) was added powdered sodium hydroxide (3.26 g) and the mixture was stirred at ambient temperature for 0.25 hours. 1-Bromo-4-chlorobutane (9.38 mL) was then added and the resulting mixture stirred at ambient temperature for 7 hours after which time TLC (ethyl acetate:dichloromethane 1:1) showed complete reaction. The reaction was poured into ice cold water (250 mL) and stirred for 0.5 hours. An oil separated and was isolated with a separatory funnel. The aqueous layer was extracted with dichloromethane (50 mL). The oil was dissolved with dichloromethane (25 mL) and the combined organics were dried with sodium sulfate, filtered and the solvent removed under vacuum. Flash chromatography (ethyl acetate:hexane, 1:1 to 2:1) yielded an oil (6.0 g) as the titled compound.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; HELTON, David; FICK, David; US2009/264443; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 3228-99-7, 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. 3228-99-7, name is Pentaerythrityl Tetrachloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In the ovenDriedNitrogen gas in a stainless steel high pressure reactor with a capacity of 75 millilitersUnder0.4 g (0.16 mmol)And tributylphosphine immobilized on chloropropyl silsesukuoxen15 g (0.13 mol) of chloroform and 52.8 g(0.39 mol) of trichlorosilane was added. Seal the reactorAfter reacting at 150 for 2 hours, the reactant was distilled under reduced pressure.18.9 g (yield 51.3%) of bis (trichlorosilyl) methane was obtained

The synthetic route of Pentaerythrityl Tetrachloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JSI Silicone Co., Ltd.; Jeong Il-nam; Kim Eun-seong; Kim Seong-min; Kim Yeong-min; (13 pag.)KR2020/15644; (2020); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 7149-75-9, name is 4-Chloro-3-methylaniline, belongs to chlorides-buliding-blocks compound, 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 7149-75-9, Product Details of 7149-75-9

tert-butyl 4-oxopiperidine-l-carboxylate (1 g, 5.02 mmol) and 4-chloro-3- methylaniline (711 mg, 5.02 mmol), were dissolved in DCE (30 mL) and acetic acid (287 mul, 5.02 mmol) was added. The reaction was stirred at 60 ¡ãC for 6 h. The reaction was allowed to cool and Sodium Tri(acetoxy)borohydride (1.49 g, 7.03 mmol) was added. The reaction was then stirred at room temperature for 18 h, then washed with water and brine. The organic layer was dried and concentrated, then purified using column chromatography (Biotage, 25g SNAP KP-SIL, 100percent DCM, 10CV). The crude product was then purified a second time using low pH reverse phase column chromatography to yield a white solid (130 mg, 8percent). LCMS Method D: rt 1.64 min, 92 percent; m/z. 269.1 (MH+-*Bu)

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.

Reference:
Patent; PRESIDENT AND FELLOWS OF HARVARD COLLEGE; EVOTEC INTERNATIONAL GMBH; GAMPE, Christian, M.; KAHNE, Daniel, Evan; KAHNE, Suzanne, Walker; QIAO, Yuan; EAST, Stephen; PARKES, Alastair, L.; SOUTHEY, Michelle; HUNTER, James; WHITTAKER, Mark; ARTHUIS, Martin; (359 pag.)WO2016/191658; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1127-85-1, 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. 1127-85-1, name is 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred suspension of INT-6 (339 mg, 1.13 mmol) in anhydrous DMF (25 mL) was added t-BuOK (1M in THF, 2.26 mL, 2.26 mmol) at 0 C. dropwise to give a brown solution. The resulting solution was stirred for further 0.5 h at this temperature. 2,4-dichloro-5,6,7,8-tetrahydroquinazoline (299.1 mg, 1.13 mmol) in DMF (5 mL) was added dropwise to the above solution and the reaction was stirred overnight at room temperature. The reaction mixture was partitioned between ethyl acetate (30 mL) and water (40 mL), the organic layer was separated and the aqueous layer was extracted with ethyl acetate (2¡Á30 mL). The combined organic layers were washed with brine (80 mL) and the organic layer was separated, dried over Na2SO4, filtered and concentrated under reduced pressure. Purification by preparative HPLC afforded I-109 (87.4 mg, 29.2%) as a yellow solid. 1H NMR (400 MHz, DMSO-d6): delta 9.34 (d, J=9.2 Hz, 1H), 8.71 (s, 1H), 8.18-8.11 (m, 2H), 7.83 (d, J=9.2 Hz, 1H), 7.58 (d, J=9.2 Hz, 1H), 7.10-7.20 (m, 1H), 3.70 (s, 2H), 3.60-3.50 (m, 1H), 3.52-3.36 (m, 6H), 2.63-2.60 (m, 2H), 2.29 (s, 3H), 1.17 (d, J=7.8 Hz, 3H), 1.06 (t, J=7.8 Hz, 3H). MS m/z (M+H): 527.0.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Celgene Avilomics Research, Inc.; Alexander, Matthew David; Chuaqui, Claudio; Malona, John; McDonald, Joseph John; Ni, Yike; Niu, Deqiang; Petter, Russell C.; Singh, Juswinder; (164 pag.)US2016/75720; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 126764-17-8, name is 1-Chloro-6,6-dimethylhept-2-en-4-yne, 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. Computed Properties of C9H13Cl

Example-6: Preparation of crystalline Form-I of Terbinafine compound of formula-3 Added 60 grams of sodium carbonate to a solution of 75 grams of N-methyl naphthylmethyl amine hydrochloride in 450 ml of water and at an ambient temperature. Stirred the reaction mixture for 45 minutes at an ambient temperature. Cooled the reaction mixture to 10-150C. Added 112.5 grams of 6,6-dimethyl-l-chlorohept-2-ene-4-yne to the above reaction mixture at 10-15C. Heated the reaction mixture to 70-750C. Stirred the reaction mixture for 6 hours at 70-750C. Cooled the reaction mixture to 25-35C. Quenched the reaction mixture with water. Extracted the reaction mixture thrice with methylene chloride. Combined all the organic phases and washed thrice with water. Separated the organic phase. Distilled the organic phase completely under reduced pressure at below 500C. Added 50 ml of isopropyl alcohol to the above reaction mixture. Distilled the solvent completely under reduced pressure at below 500C. Cooled the reaction mixture to 25-350C. Added 180 ml of isopropyl alcohol to the above reaction mixture and heated to reflux. Stirred the reaction mixture at reflux for 20 minutes. Cooled the reaction mixture to 0-50C. Stirred the reaction mixture for 60 minutes at 0-50C. Filtered the precipitated solid and washed with chilled isopropyl alcohol. Dried the material to get the crystalline Form-I of Terbinafme. Yield: 74 grams

The synthetic route of 1-Chloro-6,6-dimethylhept-2-en-4-yne has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SATYANARAYANA REDDY, Manne; RAMA SUBBA REDDY, Karamala; WO2007/96904; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, belongs to chlorides-buliding-blocks compound, 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 33050-38-3, Application In Synthesis of 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine

General procedure: Appropriate 6-chloro-[1 ,2,4]triazolo[4,3-b]pyridazine (1 eq) or 6-chloro- [1 ,2,4]triazolo[3,4-a]phtalazine (1 eq), potassium carbonate (3 to 4 eq) and the appropriate phenol, thiophenol (1 to 4 eq, 1 eq is preferentially used when R1 = CI) were dissolved in ?,?-dimethylformamide under nitrogen atmosphere. The reaction mixture was stirred overnight at room temperature or at 100-1 10C, or 5-30 minutes at 100-170C on microwave irradiation. The reaction mixture was diluted with ethyl acetate and washed with brine. The organic layer was dried over Na2S04, filtered and evaporated to dryness. The residue was purified by chromatography on silica gel, precipitated, triturated in the appropriate solvent, or used without further purification to obtain the desired 6-aryl-[1 ,2,4]triazolo[4,3-b]pyridazine, or 6-aryl-[1 ,2,4]triazolo[3,4-a]phtalazine.This protocol was used to prepare the following compounds: Cpd.1 -1 , Cpd.1 -3, Cpd.1 -4, Cpd.1 -7, Cpd.1 -8, Cpd.1 -9, Cpd.1 -10, Cpd.1 -1 1 , Cpd.1 -12, Cpd.1 -13, Cpd.1 -14, Cpd.2-1 , Cpd.2-3, Cpd.2-4 and other compounds of the invention that contain a biphenyloxy, a pyridinylphenyloxy, a thiazolylphenyloxy, or a thiopenylphenyloxy group in the 6-substituted position of the [1 ,2,4]triazolo[4,3-b]pyridazines or 6-substituted position of the [1 ,2,4]triazolo[3,4-a]phthalazine (but further information about conditions and purification are reported in Tables of Example 2).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GENFIT; BOUROTTE, Maryline; DELHOMEL, Jean-Francois; DUBERNET, Mathieu; GOUY, Marie-Helene; WO2013/45519; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1020198-58-6, These common heterocyclic compound, 1020198-58-6, name is 2-Bromo-1-chloro-3,5-difluorobenzene, 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 93 Preparation of Compound 93 (lR,4S,12aR)-N<2-chloro-4,6-dtf octahydro-l,4-methanodipyrido[l,2-a:r,2'-d]pyrazme-9-carboxarnide Step 1 A 5 mL microwave vial was charged with 2-bromo-l-chioro-3,5- difluorobenzene (540 mg, 2.4 mmol), cuprous cyanide (436 mg, 4,87 mmol), tetrakis(triphenylphosphme)palladium (63 mg, 0.05 mmol), sealed, and evacuated/backfilled with nitrogen. To this was added 5 mL degassed DMF. The sealed vessel was heated at 110 C for 18 hours, diluted with ethyl acetate, and washed sequentially with twice 9:1 NH40H:NH4Ci aq twice 5% LiCl(aq ), and brine. The organic phase was then dried over magnesium sulfate, filtered, and concentrated. The crude residue was purified by flash chromatography (100% hexanes) to afford 2-chloro-4,6- difiuorobenzonitrile. - MR (400 MHz, Chloroform-*/) delta 7.13 (dt, J ------- 8.0, 1.9 Hz, 1H), 6.93 (td, J = 8.5, 2.3 Hz, 1H). The synthetic route of 1020198-58-6 has been constantly updated, and we look forward to future research findings. Reference:
Patent; GILEAD SCIENCES, INC.; JIN, Haolun; LAZERWITH, Scott, E.; MARTIN, Teresa, Alejandra, Trejo; BACON, Elizabeth, M.; COTTELL, Jeromy, J.; CAI, Zhenhong, R.; PYUN, Hyung-Jung; MORGANELLI, Philip, Anthony; JI, Mingzhe; TAYLOR, James, G.; CHEN, Xiaowu; MISH, Michael, R.; DESAI, Manoj, C.; WO2014/100323; (2014); A1;,
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Chlorides – an overview | ScienceDirect Topics