Category: chlorides-buliding-blocks

Related Products of 50638-47-6, 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. 50638-47-6, name is 4-Bromo-2-chloro-1-methoxybenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

B. Ethyl 1-ethyl-7-(3-chloro-4-methoxyphenyl)-6,8-difluoro-1,4-dihydroquinol-4-one 3-carboxylate 300 mg (35.5% yield) was prepared by the method of Example 2 using 1.11 g 4-bromo-2-chloroanisole, 5 ml 2M t-butyl lithium solution, 750 mg zinc chloride and 720 mg ethyl 7-bromo-6,8-difluoro-1-ethyl-1,4-dihydroquinol-4-one 3-carboxylate and 100 mg tetrakis(triphenylphosphine)palladium. A yellow solid of m.p. 280 C. was recovered. NMR (CDCl3, 250 MHz): 8.45 (s, 1H), 8.15 (dd, 1H, J=2 Hz and 9 Hz), 7.55 (s, 1H), 7.4 (m, 1H), 7.1 (d, 1H, J=9 Hz), 4.4 (2q, 4H), 4.0 (s, 3H), 1.55 (t, 3H, J=6.5 Hz), 1.45 (t, 3H, J=6.5 Hz). Anal.: Calcd. for C21H18C1F2NO4.0.5H20: C, 58.00; H, 4.41; N, 3.25%. Found: C, 59.06; H, 4.52; N, 3.17%.

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-chloro-1-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Pfizer Inc.; US4623650; (1986); A;,
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Adding a certain compound to certain chemical reactions, such as: 13078-79-0, name is 2-(3-Chlorophenyl)ethanamine, 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 13078-79-0, Formula: C8H10ClN

General procedure: To a solution of morpholine (0.115 g, 1.321 mmol) in toluene (5 mL) DABAL-Me3 (0.406 g. 1.321 mmol) was added. The mixture was stirred for 20 min at 40 C. 4a (0.250 g, 1.100 mmol) were added and allowed to stir for 2 h at 90 C. The reaction mixture was quenched by the addition of 1M HCl (4 mL) and extracted with CH2Cl2 (2 × 20 mL). The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was then purified by flash column chromatography on silica gel with hexane-EtOAc as eluent to afford the desired product 6a (0.213 g, 94 %).

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-(3-Chlorophenyl)ethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kang, Soosung; Kim, Hee-Kwon; Tetrahedron; vol. 74; 30; (2018); p. 4036 – 4046;,
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Application of 81927-55-1, 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. 81927-55-1 name is Benzyl 2,2,2-trichloroacetimidate, 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.

A stirred solution of (S)- methyl 3-hydroxy-2-methylpropanoate (9.60 g, 81.3 mmol) and benzyl 2,2,2- trichloroacetimidate (22.57 g, 89.4 mmol) in CH2Cl2 (14 mL) was cooled to 0 0C under N2. Triflic acid (0.1 mL) in CH2CI2 (1 mL) was added dropwise. After 10 minutes the reaction became a solid mass. After 1 hour, saturated aqueous NaHCO3 was added and the mixture extracted with Et2O. The organics were dried over MgSO4, filtered and concentrated on a rotary evaporator. Hexane was added and the resulting solids collected by vacuum filtration. The filtrate was concentrated on a rotary evaporator and purified using flash chromatography (5-10% EtOAc/hexane) to give 11.82 g (70%) of (S)-methyl 3-(benzyloxy)-2- methylpropanoate as a colorless oil. Rf= 0.20 (10% EtOAc/hexane). 1H NMR (300 MHz, DMSO-D6) delta ppm 1.08 (d, J=7.14 Hz, 3 H) 2.75 (ddd, J=14.01, 12.64, 7.14 Hz, 1 H) 3.44 – 3.59 (m, 2 H) 3.60 (s, 3 H) 4.46 (s, 2 H) 7.23 – 7.40 (m, 5 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Benzyl 2,2,2-trichloroacetimidate, and friends who are interested can also refer to it.

Reference:
Patent; SIGNAL PHARMACEUTICALS, LLC; WO2007/84560; (2007); A2;,
Chloride – Wikipedia,
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Application of 19752-55-7, A common heterocyclic compound, 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, molecular formula is C6H3BrCl2, 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 3 In the reactor of Example 1, each chlorination of 1-bromo-3,5-dichlorobenzene was chlorinated under the specific condition. The starting materials were respectively preheated at 300 C. and 1-bromo-3,5-dichlorobenzene was fed at a rate of 7.7 g./min. and chlorine was fed at a rate of 550 ml./min. into the reactor. The reaction was continuously carried out at a reaction temperature of 360 C. and a residence time of 14 seconds for 2 hours. The reaction mixture was cooled to collect 1029 g. of the mixture. The reaction mixture was distilled to recover 263 g. of bromine (recovery percent of 84%). The residue contained the object product and a small amount of bromine and it was washed in an aqueous solution of sodium thiosulfate and the product was separated under heating it by a phase separation to obtain 722.5 g. of 1,3,5-trichlorobenzene as the object product (yield of 97.2%).

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; Ishihara Sangyo Kaisha Ltd.; US4368340; (1983); A;,
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Reference of 10061-02-6, 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. 10061-02-6, name is trans-1,3-Dichloropropene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 1.22 g (0.011 mol) of (E)-1,3-dichloropropene 6, 2.07 g(0.015 mol) of K2CO3, 50 mL of anhydrous acetonitrile, and 2.88 g (0.01 mol) of 1-[bis(4-fluorophenyl)-methyl]piperazine 5 was stirred for 0.5 h at room temperature, and then for 4 h under reflux until amine 5 was completely consumed (monitoring with GLC). After cooling, the solution was filtered, and the precipitate was washed with ethyl acetate. The combined organic layers were concentrated, and the residue was purified by column chromatography (hexane-ethylacetate, 9 : 1 ? 2 : 1). Yield 3.31 g (91%), colorless crystals, mp 89C. IR spectrum, nu, cm-1: 1609, 1506,1453, 1288, 1226, 1153, 1137, 1008, 828. 1 NMRspectrum, delta, ppm: 2.43 br.s (4H, CH2N), 2.51 br.s (4H,CH2N), 3.04 d (2H, CH2CH=, J = 7.0 Hz), 4.23 s (1H,HAr2), 5.98 d.t (1H, CH2CH=, Jtrans = 13.2, 7.0 Hz),6.15 d (1H, ClCH=, Jtrans = 13.2 Hz), 6.96 t (4H, CHAr,J = 8.5 Hz), 7.28-7.38 m (4H, CHAr). 13 NMR spectrum,delta, ppm: 51.51 (2CH2N), 52.97 (2CH2N), 58.10(C1), 74.33 (HAr2), 115.13 d (4CHAr, 2JCF = 20 Hz),120.59 (C3), 129.20 d (4CHAr, 3JCF = 6.8 Hz), 129.96(C2), 138.11 (2CAr), 161.78 d (2CFAr, 1JCF = 244.2 Hz).Mass spectrum, m/z (Irel, %): 362 (0.8) [M]+, 203 (41),201 (19), 183 (30), 161 (31), 159 (100), 132 (13), 123(32), 75 (34), 56 (15), 42 (22). Mass spectrum(HRMS), m/z: 362.1348 [M]+ (calculated forC20H21ClF2N2: 362.1361).

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, trans-1,3-Dichloropropene, other downstream synthetic routes, hurry up and to see.

Reference:
Letter; Shakhmaev; Sunagatullina, A. Sh.; Zorin; Russian Journal of General Chemistry; vol. 86; 8; (2016); p. 1969 – 1972; Zh. Obshch. Khim.; vol. 86; 8; (2016); p. 1395 – 1398,4;,
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Application of 2106-04-9, A common heterocyclic compound, 2106-04-9, name is 3-Chloro-2-fluoroaniline, molecular formula is C6H5ClFN, 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 3 Step 1. A round bottom flask was charged with 1 eq of 3-chloro-2-fluoroaniline (3A), 1- methyl-2-pyrrolidinone (about 1.5 M 3 A in NMP), 2.2 eq of sodium cyanide, and 1.35 eq of nickel(II) bromide at RT under N2. The concentration was halved by the introduction of additional NMP under N2 and the solution was gently warmed to 200+/- 5C and stirred for 4 days under N2. The reaction mixture was allowed to cool to room temperature. The reaction mixture was diluted with 30 volumes of tert-butyl methyl ether (MTBE) and filtered through celite. The celite pad was then rinsed with 10 volumes of MTBE. The organics were washed with 40 volumes of brine, 2 x 40 volumes of water and 40 volumes of brine. The combined organics were dried over sodium sulfate and concentrated to afford a brown solid, which was dried under vacuum (-30 in Hg) at 400C for 8 hours to afford the compound of Formula 3B (71 % yield).

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; CYTOKINETICS, INC.; WO2007/78839; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 622-86-6, These common heterocyclic compound, 622-86-6, name is (2-Chloroethoxy)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.

EXAMPLE 3 Preparation of N-n-propyl-N-2-phenoxyethyl amine Into a 1-liter glass reactor, which can withstand a pressure of 6 atmospheres, fitted with a stirrer, heat-ing mantle and a pressure gauge, were added 100 g 2-phenoxy ethyl chloride, 150 g propyl amine, 130 ml ethanol and 100 ml water. The reaction was heated to 100 C. for 5 hours, during which time the pressure increased to 2.2 atmospheres. Afterwards the mixture was cooled to 50 C. to lower the pressure, the propyl amine was distilled off, about 200 ml of 20% aqueous HCl was added and the white hydrochloride precipitated out. This afforded 133 g having a purity of 95% in a yield of 93%.

Statistics shows that (2-Chloroethoxy)benzene is playing an increasingly important role. we look forward to future research findings about 622-86-6.

Reference:
Patent; Makhteshim Chemical Works Ltd.; US5093526; (1992); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 1008361-80-5, name is 4-Bromo-3-chlorobenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 4-Bromo-3-chlorobenzene-1,2-diamine

Compound 14 was prepared following the procedure from Reddy and Reddy (Chem. Pharm. Bull 2010, 58, 953-956): a heterogeneous mixture of 4-bromo-3-chlorobenzene- 1,2-diamine (0.2 g) and (S)-lactic acid in 4N aq. HC1 (2 mL) was refluxed for 16 hours. The reaction mixture was then cooled to room temperature and neutralized with aq. ammonia. The resulting heterogeneous reaction mixture was extracted with EtOAc. The organic layer was dried (Na2S04) and concentrated. The residue was purified by column chromatography (silica gel, 0- 3.5 % MeOH in DCM) to afford the title compound as an orange yellow solid.

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 1008361-80-5.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAL, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; GREENLEE, William; (447 pag.)WO2017/35408; (2017); A1;,
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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. 6223-78-5, name is 2,5-Dichloro-2,5-dimethylhexane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 6223-78-5

Into a 100-mL round-bottom flask, was placed methylbenzene (60 ml_), 2, 5- dichloro-2, 5-dimethylhexane (5 g, 27.30 mmol, 1.00 eq.). This was followed by the addition of AICI3 (2.7 g, 20.48 mmol, 0.75 eq.) in several portions at 0C. The resulting solution was stirred for 1 h at room temperature. The reaction mixture was cooled to 0 C. The reaction was then quenched by the addition of 30 ml_ of water. The resulting solution was extracted with 2×50 ml_ of ethyl acetate and the organic layers combined. The resulting mixture was washed with 1 x50 ml_ of brine and dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column with EtOAc/petroleum ether (1/5). This resulted in 6.6 g (crude) of 1 , 1 ,4,4,6-pentamethyl-1 ,2,3,4-tetrahydronaphthalene as light yellow oil.

The synthetic route of 6223-78-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DAWN SCIENTIFIC PHARMACEUTICALS, LLC; TSAI, Donald; KAELIN, David; (60 pag.)WO2019/169270; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, Recommanded Product: Methyl 2,2,2-trichloroacetimidate

Step 4: Synthesis of methyl 1-{3-[(tert-butoxycarbonyl)amino]propyl}-2-(trichloromethyl)-1H-benzimidazole-6-carboxylate To a stirred solution of methyl 4-amino-3-({3-[(tert- butoxycarbonyl)amino]propyl}amino)benzoate (4.7 g, 14.5 mmol) in acetic acid (50 mL) is added methyl trichloroacetimidate (3.1 g, 17.4 mmol). After 3 h at room temperature, the solvent is evaporated, the residue is dissolved in EtOAc, and is washed with Na2C03 and brine. The organic layer is dried (Na2S04) and evaporated. The residue is triturated with hexanes to afford the title compound (5.2 g, 80%) as a fine powder. LCMS (Method T), 1.85 min, 450.63 (MH+).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2,2,2-trichloroacetimidate, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOYER, Stephen, James; BURKE, Jennifer; GUO, Xin; KIRRANE JR., Thomas, Martin; SNOW, Roger, John; ZHANG, Yunlong; WO2011/71725; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics