Chlorides-buliding-blocks

The chemical industry reduces the impact on the environment during synthesis 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, I believe this compound will play a more active role in future production and life. 60811-21-4

A solution of tert-butyl-piperazine-l-carboxylate (1.0 g, 5.37 mmol), 4-bromo-2- chloro-l-fluorobenzene (1.35 g, 6.44 mmol), t-BuONa (768 mg, 8.06 mmol), BINAP (125 mg, 0.2 mmol), Pd2(dba)3 (92 mg, 0.1 mmol) in dry toluene (10 mL) was stirred under N2 at 80C for 16 hrs. The reaction mixture was concentrated and the mixture was purified by chromatography (silica, EtOAc/PE = 1/10) to afford ter/-butyl-4-(3-chloro-4-fluorophenyl)piperazine-l- carboxylate (1.3 g, 4.13 mmol, 77%) as a yellow oil. ESI-MS (EI+, m/z): 259 [M-55]+.

The chemical industry reduces the impact on the environment during synthesis 60811-21-4. I believe this compound will play a more active role in future production and life.

Reference:
Patent; NAVITOR PHARMACEUTICALS, INC.; O’NEILL, David John; SAIAH, Eddine; KANG, Seong Woo Anthony; BREARLEY, Andrew; BENTLEY, Jonathan; (184 pag.)WO2018/89493; (2018); A1;,
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The chemical industry reduces the impact on the environment during synthesis 627-42-9, name is 2-Methoxyethyl chloride, I believe this compound will play a more active role in future production and life. 627-42-9

To a solution of 3,4-dihydroxybenzaldehyde (10 g, 72.5 mmol) (Aldrich) in DMF (200 mL) was added 2-chloroethyl methyl ether (16.5 mL, 181.2 mmol) (Aldrich), potassium carbonate (50 g, 362.3 mmol) and a catalytic amount of potassium iodide (Aldrich). The reaction mixture was heated at 85 C. for 14 hours. The reaction mixture was cooled down, diluted with EtOAc and washed with brine. The organic phase was dried over anhydrous sodium sulfate, evaporated to afford 3,4-bis-(2-methoxy-ethoxy)-benzaldehyde as an oil and was used in the next step without further purification. (Yield 11 g, 70%).

The chemical industry reduces the impact on the environment during synthesis 627-42-9. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Dominique, Romyr; Luk, Kin-Chun; Qiao, Qi; Rossman, Pamela Loreen; US2012/184548; (2012); A1;,
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The chemical industry reduces the impact on the environment during synthesis 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, I believe this compound will play a more active role in future production and life. 13918-92-8

To 5-bromo-2-methoxy pyridine-3-amine (6.3g, 31mmol) pyridine (25 ml) is added to solution of 2,4-difluoro-1-sulfonyl chloride (16.47g, 77 . 5mmol). Reaction liquid in 23 C stirring 24 hours, concentrated under reduced pressure, the volume of the solution to the original 1/2. Filtering, collecting solid, solid with i-PrOH (5mLx2) and Et 2 O (5 ml) washing. The resulting solid and NaOH (2.48g, 62mmol) suspended in MeOH (25 ml) in, the reaction solution 23 C stirring 1 hour, concentrated under reduced pressure. For residual DCM (20 ml) and 2M hydrochloric acid (20 ml) is diluted, by 5% NaHCO 3 pH7 aqueous solution is adjusted to the rear, with DCM (20mLx3) extraction. Merger of the first organic phase and the salt water (20 ml) washing, anhydrous Na 2 SO 4 drying, and concentrating under reduced pressure, to obtain the title compound as a buff solid (8.2g, 69.9%).

The chemical industry reduces the impact on the environment during synthesis 13918-92-8. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Guangdong East Sunshine Pharmaceutical Co., Ltd. / Sunshine Lake Pharma Co., Ltd; Jiata Science company; Xi, Ning; Li, Zhuo; Wang, Tingjin; Wu, Zuping; Wen, Qiuling; (65 pag.)CN103539777; (2016); B;,
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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. 627-42-9, name is 2-Methoxyethyl chloride, A new synthetic method of this compound is introduced below., 627-42-9

General procedure: NaBH4 (23 mg, 0.60 mmol, 3.0 eq.) was portionwise added to a solution of 4,4′-diselanediyldibenzenesulfonamide 1 (94 mg, 0.20 mmol, 1.0 eq.) in EtOH (2 mL) at 0 C under inert atmosphere (N2). After 30 min, the halo-alkyl 2a-f (0.36 mmol, 2.1 eq.) was slowly added and the reaction mixture was stirred at reflux for 3 h, until complete consumption of the starting material was observed by TLC. The reaction was quenched by addition of saturated aq. NH4Cl (2 mL) and diluted with EtOAc (5 mL). The layers were separated and the aqueous layer was extracted with EtOAc (2 x 5 mL), dried over Na2SO4, filtered and concentrated under vacuum. The crude material was purified by flash chromatography to yield selenides (3a-f) bearing benzenesulfonamide moiety.

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:
Article; Angeli, Andrea; di Cesare Mannelli, Lorenzo; Lucarini, Elena; Peat, Thomas S.; Ghelardini, Carla; Supuran, Claudiu T.; European Journal of Medicinal Chemistry; vol. 154; (2018); p. 210 – 219;,
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Adding some certain compound to certain chemical reactions, such as: 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, 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 6579-54-0. 6579-54-0

General procedure: A mixture of N-Boc-aminol (1 eq.) and KOH (3eq) in THF was stirred vigorously for 15 min. It was followed by the addition of required benzenesulfonyl chloride derivative (1.2eq) and subsiquent stirring of the reaction for 4-5h. After completion of the reaction (as per TLC), the reaction mixture was filtered to expel out the precipitated salt and the filterate thus obtained was concentrated under reduced pressure to obtain the crude product which was further purified by column chromatography (eluent EtOAc:Hexane).

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 2,6-Dichlorobenzenesulfonyl chloride.

Reference:
Article; Saxena, Anil K.; Sharma, Sugandha; Pandey, Atindra K.; Shukla, Praveen K.; Bioorganic and Medicinal Chemistry Letters; vol. 21; 21; (2011); p. 6476 – 6481;,
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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. 112-26-5 name is 1,2-Bis(2-chloroethoxy)ethane, 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. 112-26-5

8-(9-chloro-1,4,7-trioxanon-1-yl) quinoline 8-hydroxyquinolinoe (1 g, 6.89 mmol) and potassium carbonate (1.43 g, 10.33 mmol) was stirred at room temperature in CH3CN for 2 h. The solution of 1,2 bis(2-chloroethoxy)ethane (2.58 g, 13.79 mmol) was added and the mixture was refluxed for 48 h. The solid residue was removed by filtration over filter paper. Then the filtrate was evaporated to dryness under rotary evaporator to yield brown oil. This was further purified by column chromatography through silica gel (EA/heaxane, 1:2) to give 8-(9-chloro-1,4,7-trioxanon-1-yl) quinoline as pale straw coloured oil (0.82 g, 40% yield). 1H NMR (500 MHz, CDCl3, 298 K): delta=8.89 (dd, J (H,H)=4 Hz, 1H, qu-CH), 8.10 (dd, J (H,H)=6 Hz, 1H, qu-CH), 7.39 (m, 3H, qu-CH), 7.07 (d, 1H, J (H,H)=8 Hz, qu-CH), 4.38 (t, 3J (H,H)=5 Hz, 2H, CH2), 4.05 (t, 3J (H,H)=5 Hz, 2H, alpha-CH2), 3.74 (m, 6H, CH2), 3.59 (t, 3J (H,H)=5 Hz, 2H, CH2).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,2-Bis(2-chloroethoxy)ethane, and friends who are interested can also refer to it.

Reference:
Patent; National Dong Hwa University; LIN, Ivan Jyh Biau; HSU, Tina H. T.; CHOU, Shiu-Huey; (19 pag.)US2017/129907; (2017); A1;,
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A common compound: 13726-14-2, name is 4-Chloro-3-methoxyaniline, belongs to chlorides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 13726-14-2

Into a vessel containing 3 mL of dioxane was added 60 mg of Exp-5-g24 prepared in Step 2 (0.19 mmol), 31 mg of 4-chloro-3-methoxy-phenylamine (0.2 mmol), 18 mg of Pd2dba3 (0.02 mmol), 23 mg of Xantphos (0.04 mmol) and 130 mg Cs2C03 (0.4 mmol). The reaction mixture thus provided was maintained under an 2 atmosphere, refluxed for 3 hours, then cooled to ambient temperature, filtered and concentrated under reduced pressure. The residue thus provided was purified by Prep-TLC (PE:EtOAc = 1 :2) yielding 65 mg of Exp-5-g25 (calculated yield 70 %).

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, 13726-14-2, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; LIVERTON, Nigel; JONES, Philip; LEI, Zhiyu; LIU, Fuqing; LUO, Yunfu; DONG, Jingchao; SOLL, Richard; WO2013/63100; (2013); A1;,
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118-69-4, Adding a certain compound to certain chemical reactions, such as: 118-69-4, name is 2,6-Dichlorotoluene, 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 118-69-4.

Ammoxidation runs were carried out in a fixed bed tubular quartz reactor, which is filled with 5g of catalyst particles prepared by the methods described in examples 1 to 3 and mixed with corundum particles of the same size in 1: 1 by weight ratio. A preheating zone is provided on the top of the catalyst bed. The catalyst was activated in a mixture of air and [NH3] at [400C] for 4 hours and then the catalytic runs were performed. The 2,6-DCT and [H20] were pumped in the mole ratio of 1: 15 to 20. The product stream was collected for every half-an-hour and analysed by gas chromatography. The reaction was carried out under the following reaction conditions. A reaction temperature of 350 to [400C] was used, and the GHSV comprised between 650-750 [H-‘.] The contact time consisted of 4.8 to 5.5 seconds. The mole ratio of 2,6-DCT : H20 : NH3: air was 1: 15: 3-4: 21, the molar concentration of 2,6-DCT was 2.4 % and the ratio of O/NH3 was 1. [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, 2,6-Dichlorotoluene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TESSENDERLO CHEMIE S.A.; WO2003/101939; (2003); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding some certain compound to certain chemical reactions, such as: 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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 41965-95-1. 41965-95-1

tert-butyl 8-bromo-10-((3-chloro-4-methoxybenzyl)amino)-3,4-dihydrobenzo[b][1,6]naphthyridine-2(1H)-carboxylate, 21 A mixture of 20 (0.075 mmol), 3-chloro-4-methoxybenzyl amine hydrochloride (0.38 mmol), TEA (0.38 mmol) and NaI (0.0037 mmol) in NMP (1 mL) was heated to 130 C. and stirred overnight. The reaction was diluted with Et2O (10 mL) and washed with H2O (2*20 mL) and brine (20 mL). The organic layers were dried over Na2SO4, filtered and evaporated under reduced pressure to give the desired intermediate 21 (40% yield). 1H NMR (300 MHz, CDCl3) delta 8.08 (s, 1H), 7.84 (s, 1H), 7.68 (d, 1H, J=9.0 Hz), 7.35 (s, 1H), 7.19 (d, 1H, J=8.1 Hz), 6.93 (d, 1H, J=8.1 Hz), 4.57 (s, 4H), 3.91 (s, 3H), 3.76 (t, 2H, J=6.0 Hz), 3.19 (t, 2H, J=5.7 Hz), 1.49 (s, 9H).

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 3-Chloro-4-methoxybenzylamine Hydrochloride.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; Landry, Donald W.; Deng, Shixian; Arancio, Ottavio; Fiorito, Jole; Wasmuth, Andrew; (41 pag.)US10626113; (2020); B2;,
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A common heterocyclic compound, 2770-11-8, name is 2-(4-Chlorophenoxy)aniline, molecular formula is C12H10ClNO, 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. 2770-11-8.

To a stirred and cooled solution of 2-(4-chlorophenoxy)aniline (330 mg, 1.50 mmol) and triethylamine (230 muL, 1.65 mmol) in toluene (5 mL), the appropriate acid chloride (pivaloyl chloride, 2,2-dimethylbutyryl chloride, 3-methylbutyryl chloride, propyl chloride, cyclopropanecarbonyl chloride, cyclobutanecarbonyl chloride, methyl succinyl chloride, 4-methoxybenzoyl chloride) (1.65 mmol) was added. Subsequently the reaction mixture was allowed to warm to room temperature. The progress of the reaction was monitored by TLC. After 2-9 h the reaction mixture was extracted with a saturated sodium hydrogen carbonate solution, with a hydrogen chloride solution (10%), with brine and finally with water. Afterwards the organic solution was dried over sodium sulfate and evaporated under reduced pressure. The residue was further purified by recrystallization or column chromatography over silica gel. N-[2-(4-Chlorophenoxy)phenyl]-2,2-dimethylpropanamide (1): Crystallization from ethanol (70%) yielded slightly brown needles (277 mg, 0.92 mmol, 61%); m.p.: 99-100 C ; IR (KBr): [cm-1] nu = 3336 (br, N-H), 1663 (s, C=O); 1H-NMR: (400 MHz, DMSO-d6) delta [ppm] = 1.05 (s, 9H, C(CH3)3), 6.80-7.01 (m, 2H, arom. H), 6.99-7.15 (m, 1H, arom. H), 7.15-7.32 (m, 2H, arom. H), 7.27-7.48 (m, 2H, arom. H), 7.56-7.78 (m, 1H, arom. H), 8.72 (s, 1H, NH); 13C-NMR: (101 MHz, DMSO-d6) delta [ppm] = 26.95 (3C, CH3), 118.40 (2C), 120.46, 124.63, 126.13, 126.62, 129.49 (2C) (CH), 38.12, 126.38, 130.28, 147.84, 155.91 (C), 176.13 (C=O); C17H18ClNO2 (303.78): calcd. C 67.21, H 5.97, N 4.61, found C 67.13, H 6.00, N 4.51; EI-MS: m/z (%): 303.1 [M]+ (28), 176.1 [M – 127]+ (100); HPLC: 99.7% at 254 nm, 99.9% at 280 nm; tR = 7.42 min, tM(DMSO) = 1.06 min (ACN/H2O 60:40), lambdamax [nm] = 230, 275; HPLC-gradient: 99.4%, tR = 13.62 min, tM(DMSO) = 1.28 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(4-Chlorophenoxy)aniline, its application will become more common.

Reference:
Article; Weidner, Thomas; Nasereddin, Abed; Preu, Lutz; Gruenefeld, Johann; Dzikowski, Ron; Kunick, Conrad; Molecules; vol. 21; 2; (2016);,
Chloride – Wikipedia,
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