Tag: M.W=200-300

Synthetic Route of 1940-29-0, 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. 1940-29-0 name is 4-Bromo-3,5-dichloroaniline, This 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.

(4-Bromo-3,5-dichloro-phenyl)-[5-methanesulfonyl-2-(4-methoxy-benzyl)-2H- [l,2,4]triazol-3-yl]-amine In a 25 mL round bottle, 5-chloro-l-(4-methoxybenzyl)-3-(methylsulfonyl)-lH-l,2,4-triazole (200 mg, 663 muiotaetaomicron, Eq: 1.00) was combined with DMF (3 mL) to give a colorless solution. 4- Bromo-3,5-dichloroaniline (160 mg, 663 muiotaetaomicron, Eq: 1.00) and sodium 2-methylpropan-2-olate (127 mg, 1.33 mmol, Eq: 2.00) were added. The reaction was degassed by nitrogen for 5 min. The resulting solution was heated to 85 C overnight under nitrogen. The reaction mixture was cooled and diluted with 20 mL H20, added Ether (30×2 mL) to extract the product, dried the organic layer over anhydrous Na2S04, concentrate the solution, purify the compound by column (Hexanes/EtOAc = 70/30) to afford the compound 180mg (54%). MH+ 507.0

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-3,5-dichloroaniline, and friends who are interested can also refer to it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; DING, Qingjie; JIANG, Nan; WEIKERT, Robert James; WO2014/135472; (2014); 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. 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

A 100 mL 3 -neck flask was placed under N2 and equipped with a condenser and an addition funnel. Magnesium (2.0 g, 83 mmol) were added, bromo-3-chloro- 5-fluoro benzene (15 g, 72.5 mmol) was taken up in dry THF (70 mL), and transferred to the addition funnel. The Grignard reaction was initiated with approximately 2 mL of the bromo-3-chloro -5-fluorobenzene solution and iodine. The remaining bromo-3-chloro-5-fluorobenzene solution was added and the reaction was refluxed 1 hour.

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; VITAE PHARMACEUTICALS, INC.; WO2008/156817; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 6579-54-0, The chemical industry reduces the impact on the environment during synthesis 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, I believe this compound will play a more active role in future production and life.

Synthesis Example 26 Synthesis of 2,6-Dichlorobenzenesulfonamide [Compound (III-7)] To a solution obtained by dissolving 29% aqueous ammonia (6.9 g, 20.36*5 mmol) in 40 ml of acetonitrile was added dropwise a solution of 2,6-dichlorobenzenesulfonyl chloride [Compound (XXII-7)] (5 g, 20.36 mmol) in 10 ml of acetonitrile under cooling with water. Thereafter, the reaction solution was stirred at room temperature for 3 hours and distilled off. Water was added to the residue, followed by filtration to obtain an insoluble material, which was washed with water and then with a small amount of acetonitrile. White solid, m.p.; 173-5 C., yield: 4.3 g, percent yield: 94%. IR KBr cm-1: 3382, 3268, 1575, 1428, 1338, 1143, 780. 1H-NMR (60 MHz, d6-DMSO, delta): 7.4-7.6 (3H, aromatic ring H), 7.6-7.9 (2H, bs NH2).

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, 2,6-Dichlorobenzenesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kureha Kagaku Kogyo K.K.; US6610853; (2003); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 699-89-8, name is 4,7-Dichlorothieno[2,3-d]pyridazine, molecular formula is C6H2Cl2N2S, 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. HPLC of Formula: C6H2Cl2N2S

A 250 mL, round-bottomed flask was equipped with a stir bar and reflux condenser. To the flask was added the product of step 4 (7.65 g, 37.3 mmol), 4-chloroaniline (4.76, 37.3 mmol) in EtOH (75 mL). The mixture was refluxed for 3 h. An orange solid precipitated from the reaction after 3 h. The reaction was cooled to rt and the solid was collected by filtration and washed with hexane. The desired 7-chloro-4-(4-chlorophenylamino)thieno[2,3-d]pyridazine was obtained (6.5 g, 21.9 mmol; 60% yield); mp=139-142 C.; ES MS (M+H)+=297; TLC (Hexane-EtOAc, 60:40); Rf=0.48.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 699-89-8, its application will become more common.

Reference:
Patent; Bayer Pharmaceuticals Corporation; US6689883; (2004); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 14862-52-3, The chemical industry reduces the impact on the environment during synthesis 14862-52-3, name is 3,5-Dibromochlorobenzene, I believe this compound will play a more active role in future production and life.

A solution of 1,3-dibromo-5-chlorobenzene (10 mmol, 3.2 g)Diphenylamine (40 mmol, 6.7 g) was added to a 100 mL three-necked flask,A cuprous iodide (4 mmol, 0.8 g) was added under nitrogen,Potassium carbonate (40 mmol, 2.8 g),Phenanthroline (4 mmol, 0.8 g),50 mL of DMF,The reaction was carried out at 155 C for 3 days,The resulting reaction product is subjected to extraction,The extracted organic phase was evaporated to dryness with ethanol,And then recrystallized from ethyl acetate and petroleum ether to give 3.57 g of intermediate A-4,

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, 3,5-Dibromochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jilin Aolai De Optoelectronic Materials Co., Ltd.; Gao, Chunji; Cui, Dunzhu; Sun, Yi; Zhang, Chengcheng; (52 pag.)CN104892434; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 928783-85-1, These common heterocyclic compound, 928783-85-1, name is 1-Bromo-3-chloro-5-(trifluoromethyl)benzene, 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.

In a 25 mL sealed tube, sodium 2-methylpropan-2-olate (62.7 mg, 653 muetaiotaomicron, Eq: 1.20), bis(dibenzylideneacetone)palladium (31.3 mg, 54.4 muetaiotaomicron, Eq: 0.1) and 2-di-tert-butyl(2′,4′,6′- triisopropylbiphenyl-2-yl)phosphine (23.1 mg, 54.4 muetaiotaomicron, Eq: 0.1) were combined with toluene (5.00 mL) to give a dark brown suspension. N5,N5,l-tris(4-methoxybenzyl)-lH-l,2,4-triazole- 3,5-diamine (250 mg, 544 muetaiotaomicron, Eq: 1.00) and l-bromo-3-chloro-5-(trifluoromethyl)benzene (141 mg, 544 muetaiotaomicron, Eq: 1.00) were added. The reaction mixture was degassed with argon for 15 min, and then heated to 110C for 3 hours. The reaction mixture was cooled and diluted with EtOAc (50 mL), washed with H20 (25 mL) and brine (25 mL). The organic layer was dried over anhydrous MgS04, filtered and volatiles were removed under reduced pressure to yield an oil from which the compound was isolated by column chromatography (Hexanes/EtOAc = 70/30) to give an off-white solid 40 mg (12%). MH+ 638.4

Statistics shows that 1-Bromo-3-chloro-5-(trifluoromethyl)benzene is playing an increasingly important role. we look forward to future research findings about 928783-85-1.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BILOTTA, Joseph Anthony; CHEN, Zhi; CHIN, Elbert; DING, Qingjie; ERICKSON, Shawn David; GABRIEL, Stephen Deems; KLUMPP, Klaus; MA, Han; MERTZ, Eric; PLANCHER, Jean-Marc; WEIKERT, Robert James; WO2014/6066; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 3386-33-2,Some common heterocyclic compound, 3386-33-2, name is 1-Chlorooctadecane, molecular formula is C18H37Cl, 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.

After dropping 173.4 g (0.6 mol) of 1-chlorooctadecane thereinto within about 15 minutes, the mixture was allowed to stand overnight under stirring at room temperature. Then the reaction mixture was washed with 500 ml of isopropyl ether and thus crystals of acryloyloxyethyl-N,N-dimethyloctadecylammonium chloride were obtained.

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

Reference:
Patent; Hisamitsu Pharmaceutical Co, Inc.; US5665348; (1997); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 328-72-3, 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. 328-72-3 name is 3,5-Bis(trifluoromethyl)chlorobenzene, This 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.

STR7 Preparation of 3,5-bis-(trifluoromethyl)-benzonitrile By the method of Example 3, 124 g of 1-chloro-3,5-bis-(trifluoromethyl)-benzene in 120 ml of ethyl methyl ketone gave 61.4 g (51.2% of theory) of 3,5-bis-(trifluoromethyl)-benzonitrile (b.p.45 mbar: 88 C.). After 20 hours, the conversion was approximately 60%. 4.5% of coupling products had formed.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Bis(trifluoromethyl)chlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Bayer Aktiengesellschaft; US6162942; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 38762-41-3, The chemical industry reduces the impact on the environment during synthesis 38762-41-3, name is 4-Bromo-2-chloroaniline, I believe this compound will play a more active role in future production and life.

Description 13; (4-Bromo-2-chlorophenyl)-(tetrahydropyran-4-yl)-amine (D13); A mixture of 4-bromo-2-chloro-phenylamine (0.5 g, 2.422 mmol), tetrahydropyran-4- one (1.308 ml, 10.898 mmol), and sodium triacetoxyborohydride (2.31 g, 10.898 mmol) in DCE (20 ml) was stirred at room temperature for 16 h. The reaction mixture was washed with NaHCO3 (aqueous sat. solution), dried (Na2SO4) and the solvent was evaporated in vacuo. The residue was purified by column chromatography (silica gel; heptane/DCM up to 40% as eluent). The desired fractions were collected and evaporated in vacuo to yield compound D13 (0.383 g, 52%) as white solid. LCMS: MW (theor): 289; [MH+]: 290; RT (min): 4.39 (Method 1).

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, 4-Bromo-2-chloroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ORTHO-MCNEIL-JANSSEN PHARMACEUTICALS, INC.; ADDEX PHARMA S.A.; CID-NUNEZ, Jose, Maria; TRABANCO-SUAREZ, Andres, Avelino; MACDONALD, Gregor, James; WO2010/60589; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 933190-51-3 as follows. Safety of 8-Bromo-6-chloroimidazo[1,2-b]pyridazine

A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser was charged with 104a (2.0 g, 4 mmol), 5-(4-methylpiperazin-1-yl)pyridin-2-amine (920 mg, 4.8 mmol), tris(dibenzylideneacetone)dipalladium(0) (366 mg, 0.4 mmol), XantPhos (688 mg, 1.2 mmol), Cs2CO3 (2.6 g, 8.0 mmol), and 1,4-dioxane (60 mL). After three cycles of vacuum/argon flush, the mixture was heated at reflux for 15 h. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica-gel column chromatography eluting with dichloromethane/methanol (20:1) to afford 104b as yellow solid (1.4 g, 70%). MS: [M+H]+344.

According to the analysis of related databases, 933190-51-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GENENTECH, INC.; Crawford, James John; Ortwine, Daniel Fred; Young, Wendy B.; US2013/116262; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics