Tag: M.W=100-200

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;,
Chloride – Wikipedia,
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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,
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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;,
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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;,
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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;,
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Synthetic Route of 106-39-8, 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 106-39-8 as follows.

The reaction of 1-bromo-4-chlorobenzene(0.191 g, 1.0 mmol), aniline (0.093 g, 1.0 mmol), copper powder (0.0064 g, 0.1mmol), MI (0.036 g, 0.2 mmol), Cs2CO3 (0.720 g, 2.2 mmol), TBAHS (0.068 g, 0.2mmol) produced 0.146 g (72%) of 4-chloro-N-phenylaniline as an brown solid.

According to the analysis of related databases, 106-39-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhou, Qifan; Du, Fangyu; Chen, Yuanguang; Fu, Yang; Chen, Guoliang; Tetrahedron Letters; vol. 60; 29; (2019); p. 1938 – 1941;,
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Reference of 432-21-3, 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 432-21-3 as follows.

To a stirred solution of chloral hydrate (2.54 g, 15.3 mmol) in H20 (30 ml) was addedNa2S04 (0.87 g, 6.14 mmol) and 3-chloro-2-(trifluoromethyl)aniline (2.00 g, 10.2 mmol)followed by addition of NH20H.HCI (2.13 g, 30.7 mmol) at room temperature. The reactionmixture was heated at 55C for 16h. Progress of reaction was monitored by TLC and5 LCMS. After completion, the reaction mixture was diluted with H20 (1 00 ml) andextracted with EtOAc (2 x 40 ml). The organic layer was separated, dried over anhydrousNa2S04 and concentrated under vacuum. The crude obtained was purified by combi-flashchromatography (10 to 20% EtOAc in hexanes) to (E)-N-(3-chloro-2-(trifluoromethyl)phenyl)-2-(hydroxyimino)acetamide Xl-16a (1.25 g) as an off-white solid.10 Yield: 44%.Basic LCMS Method 2 (ES-): 265 (M-H)-, 97 % purity.1H NMR (400 MHz, DMSO-d5) o 7.48 (d, J=7.82 Hz, 1 H) 7.61 (s, 1 H) 7.62-7.68 (m, 2H)10.10 (s, 1H) 12.36 (s, 1H).

According to the analysis of related databases, 432-21-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UCB PHARMA GMBH; MUELLER, Christa E.; PEGURIER, Cecile; DELIGNY, Michael Louis Robert; EL-TAYEB, Ali; HOCKEMEYER, Joerg; LEDECQ, Marie; MERCIER, Joel; PROVINS, Laurent; BOSHTA, Nader M.; BHATTARAI, Sanjay; NAMASIVAYAM, Vigneshwaran; FUNKE, Mario; SCHWACH, Lukas; GOLLOS, Sabrina; VON LAUFENBERG, Daniel; BARRE, Anais; (493 pag.)WO2018/122232; (2018); A1;,
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Related Products of 78068-85-6, 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. 78068-85-6, name is 3-Chloro-4-fluorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 1-benzofuran-6-ol (418.5 mg, 3.1 mmol) in 6 ml of DMF was added 3-Chloro-4-fluorobenzotrifluoride (681.4 mg, 3.4 mmol) and cesium carbonate (1.5 g, 4.7 mmol). The reaction mixture was heated at 80 C. for 2 hours. After cooling to room temperature, it was diluted with ethyl acetate, washed with water (2×) and brine, dried over magnesium sulfate, filtered and concentrated. The crude product was purified on a silica gel column, eluting with ethyl acetate (0-30%) in hexane. The final product was collected as colorless oil. 1H NMR (CDCl3, delta ppm): 6.8 (s, 1H), 7.0 (two d, 2H), 7.2 (s, 1H), 7.4 (d, 1H), 7.6 (d, 1H), 7.7 (s, 1H), 7.8 (s, 1H).

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-Chloro-4-fluorobenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ge, Min; He, Jiafang; Lau, Fiona Wai Yu; Liang, Gui-Bai; Lin, Songnian; Liu, Weiguo; Walsh, Shawn P.; Yang, Lihu; US2007/265332; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

72934-36-2, name is 1-(4-Chlorophenyl)cyclopropanamine, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C9H10ClN

To a slurry of tert-butyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-l,3,5-triazin-2- ylamino)benzoate (3.6 g) andl-(4-chlorophenyl)cyclopropanamine (1.49 g) in THF (50 mL) was stirred for 5 hours at 80C. The precipitate was filtrated through a plug washing with THF to give acrude product that was purified by Biotage eluting with 4/1-hexane/ethyl acetate to give 1.8 g of tert-butyl 4-(4-(l-(4- chlorophenyl)cyclopropylamino)-6-(2,2,2-trifluoroethoxy)-l,3,5-triazin-2- ylamino)benzoate as a solid.

The synthetic route of 72934-36-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WANG, Tao; ZHANG, Zhongxing; HAN, Ying; YIN, Zhiwei; SCOLA, Paul Michael; WO2014/116768; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics