Month: August 2021

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. 38762-41-3, name is 4-Bromo-2-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Bromo-2-chloroaniline

General procedure: Phenyl phenylphosphoramidochloridate (1) (0.001 mol) and 2-amino-benzothiazole (2a) (0.001 mol) were taken in a bottomed flask (50 mL) and THF (20 mL) was added. To thismixture, dimethylpiperazine (DMP) (0.001 mol) was added andthe reaction mixture was stirred vigorously at 30-50 C for 4 h.The progress of the reaction was monitored by TLC. After completionof the reaction, DMP. HCl was removed by filtration andthe filtrate was concentrated under vacuum and the resultantsolidwas purified by passing through a columnof silica gel usinghexane:ethyl acetate (2:1) as an eluent to afford title compound,phenylN-1,3-benzothiazol-2-yl-N?-phenylphosphorodiamidate(3a). The same experimental procedure was adopted for the preparation of the remaining title compounds (3b-j) (Scheme 1).

The synthetic route of 38762-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Nayab Rasool; Babu, P. Hari; Janaki Ramudu; Jyothi Kumar; Appa Rao, Ch.; Raju, C. Naga; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 193; 1; (2018); p. 10 – 13;,
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Related Products of 261762-56-5, 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 261762-56-5 as follows.

In a four-necked 250 mL round-bottomed flask, equipped with a thermometer, a reflux condenser with pressure equalizer, a dry ice cooled dropping funnel (-30 C) and a gas inlet, 50.0 g (purity 97.0 w%, 302 mmol, 1.0 eq) of l-chloro-2-fluoro-3-methoxy-benzene (1, CAS- No. 261762-56-5) were dissolved in 70 mL of chlorobenzene. To the solution 53.1 g (purity 98.0 w%, 332 mmol, 1.1 eq) bromine was added over one hour at 5-10 C internal temperature via cooling externally at 0 C. After complete addition the reaction was allowed to reach 25 C. The reaction was continued for further 8 hours under a constant stream of nitrogen purge gas to remove HBr from the reaction mixture. Afterwards a HPLC measurement indicated >98% conversion. The reaction solution was then washed with 100 mL of aqueous saturated NaHC03 solution and 50 mL of deionized water. Afterwards the organic phase was dried over MgSC^, the drying agent was filtered off and the solvent was removed in vacuum at 65 C and 5 mbar to leave 72.6 g (90%, purity 90%) of a brownish solid. The solid was purified via vacuum distillation at 10 mbar and temperature of 118-122 C to yield 57.4 g (79%, purity 99%) of a white solid. NMR (CDC13, 400 MHz) delta (ppm) = 7.34 (dd, J= 8.0, 2.0 Hz, 1H), 6.79 (dd, J= 8.0, 8.0 Hz, 1H), 3.89 (s, 3H).

According to the analysis of related databases, 261762-56-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; MUeHLTHAU, Friedrich, August; FORD, Mark, James; ERVER, Florian; BREMEYER, Nadine; PLATZEK, Johannes; GUIMOND, Nicolas; BADER, Thomas; ALBRECHT, Uwe; (129 pag.)WO2018/46684; (2018); A1;,
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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. 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, A new synthetic method of this compound is introduced below., COA of Formula: C13H11ClFNO

General procedure: Acetic acid (2.0 mL) and aniline derivatives (1.10mmol) was added to 6 (1.00 mmol). The mixturewas heated to 125-130 C andstirred for 15 min. The reaction mixture was then cooled to 25 C.The acetic acid was evaporated. To the reaction mixture, ice-water(10 mL) was added and adjusted pH to 9 with ammonium hydroxide.The mixture was stirred for 0.5 h. The precipitated productwas filtered, and the filtered cake was washed with water(3 x 10 mL) to afford crude product. The crude product was chromatographedby silica gel, eluting with EtOAc/petroleum ether(1:4) to afford 7a-7f (yield 82-94%) as white solid. 4.1.7.1 4-(3-chloro-4-(3-fluorobenzyloxy)phenylamino)-6,7-bis(2-chloroethoxy)quinazoline (7a) Yield: 86%. 1H NMR (600?MHz, DMSO-d6) delta(ppm): 9.47 (s, 1H), 8.48 (s, 1H), 7.97 (d, J?=?2.6?Hz, 1H), 7.91 (s, 1H), 7.71 (dd, J?=?8.9, 2.6?Hz, 1H), 7.50-7.46 (m, 1H), 7.35-7.31 (m, 2H), 7.28 (s, 1H), 7.26 (s, 1H), 7.20-7.16 (m, 1H), 5.25 (s, 2H), 4.48-4.45 (m, 4H), 4.08 (t, J?=?5.5?Hz, 2H), 4.04 (t, J?=?5.0?Hz, 2H). 13C NMR (151?MHz, DMSO-d6) delta(ppm): 162.2 (d, 1JC-F?=?243.7?Hz), 156.3, 153.2, 153.1, 149.5, 147.5, 147.0, 139.7, 139.6, 133.4, 130.5 (d, 3JC-F?=?8.3?Hz), 124.0, 123.3 (d, 4JC-F?=?2.6?Hz), 122.1, 121.1, 114.6 (d, 2JC-F?=?20.9?Hz), 114.3, 114.0 (d, 2JC-F?=?21.9?Hz), 109.0 (d, 3JC-F?=?8.6?Hz), 104.7, 69.5, 69.4, 68.9, 42.7, 42.6.

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; Zhang, Yaling; Chen, Li; Xu, Hongjiang; Li, Xiabing; Zhao, Lijun; Wang, Wei; Li, Baolin; Zhang, Xiquan; European Journal of Medicinal Chemistry; vol. 147; (2018); p. 77 – 89;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 15205-15-9, These common heterocyclic compound, 15205-15-9, name is 2-Chloro-6-fluorobenzylamine, 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.

General procedure: A mixture of 0.55mmol of 8-bromo-7-(2-bromoethyl)theophylline 7a or 8-bromo-7-(3-chloropropyl)theophylline 7b or 8-bromo-7-(4-bromobutyl)theophylline 7c, 1.1mmol of appropriate aromatic amine, 1,6 mmol of TEBA and 1.00ml of propanol was heated in closed vessels in microwave oven (300 Watt, Power Max Off, 160C, 10bar) for 1h. The solvent was removed and the residue was treated with ethanol. The products were purified by crystallization from ethanol or flash column chromatography over silica gel with CH2Cl2 : MeOH (100 : 0 to 80 : 20). The precipitate was filtered off and dried.

The synthetic route of 15205-15-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Za?uski, Micha?; Schabikowski, Jakub; Schlenk, Miriam; Olejarz-Maciej, Agnieszka; Kubas, Bart?omiej; Karcz, Tadeusz; Kuder, Kamil; Latacz, Gniewomir; Zygmunt, Ma?gorzata; Synak, David; Hinz, Sonja; Mueller, Christa E.; Kie?-Kononowicz, Katarzyna; Bioorganic and Medicinal Chemistry; vol. 27; 7; (2019); p. 1195 – 1210;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 7051-16-3,Some common heterocyclic compound, 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene, molecular formula is C8H9ClO2, 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.

To a -78 C. solution of 1-chloro-3,5-dimethoxybenzene (1.73 g, 10 mmol) in 10 mL of CH2Cl2 was added 10 mL of BBr3/CH2Cl2. The reaction mixture was stirred at -78 C. for 2 h, then allowed to warm up to RT overnight. To the mixture was added water and the product was extracted with EtOAc (3*10 mL). The combined organic layers were washed with water (10 mL) and brine (10 mL), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford a crude product. The residue was purified by flash chromatography (1:1 EtOAc/hexanes) to give 3-chloro-5-isobutoxyphenol as a yellow solid (1.23 g, 85%). MS (ES+) C6H5ClO2 requires: 144. found: 145 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-3,5-dimethoxybenzene, its application will become more common.

Reference:
Patent; Board of Regents, The University of Texas System; Palmer, Wylie; Jones, Philip; Liu, Gang; Petrocchi, Alessia; Reyna, Naphtali; Subrumanian, Govindan; Theroff, Jay; Yau, Anne; (114 pag.)US2016/60260; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 6223-78-5, A common heterocyclic compound, 6223-78-5, name is 2,5-Dichloro-2,5-dimethylhexane, molecular formula is C8H16Cl2, 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.

1,1,4,4,6-pentamethyl-1,2,3,4-tetrahydronaphtalene 4: To a solution of 2,5 dichloro-2,5 dimethylhexane 2 (10 g, 54.7 mmol) in toluene (270 Ml, 0.2 M) is slowly added aluminum trichloride (5.47 g, 41 mmol) as a solid over a 15-minute period. The reaction is complete after 10 minutes as assayed by tlc in hexanes. The unreacted aluminum trichloride is quenched slowly with water over 10 minutes. Additional toluene (250 mL) is added to extract the product from the aqueous layer. The organic layer is passed through a pad of silica gel (40 g) and eluted with toluene. The organic layer is evaporated in vacuo to dryness to yield 1,1,4,4,6-pentamethyl-1,2,3,4-tetrahydronaphtalene 4 (11 g, 97% yield). NMR 1.29 (s, 6H), 1.28 (s, 6H), 1.69 (s, 4H), 2.32 (s, 3H), 7.22 (d, 1H), 7.12 (s, 1H), 6.97 (dd, 1H).

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; Pfizer Inc.; US2004/10033; (2004); 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. 2106-02-7, name is 2-Chloro-4-fluoroaniline, A new synthetic method of this compound is introduced below., Safety of 2-Chloro-4-fluoroaniline

General procedure: A solution of salicylaldehyde derivative (1.0 equiv.) in ethanol (5.0 mL mmol-1)was added into a solution of aniline derivative (1.0 equiv.) in ethanol (5.0 mL mmol-1). After stirring at room temperature for 1 h, the mixture was refluxed until complete consumption of the starting materials. Subsequently, ethanol was removed under reduced pressure and the obtained imines were purified by crystallization. The obtained Schiff-bases were characterized by NMR and elemental analysis. All analytical data is in accordance with literature [21,26,30,32,33,43].

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; Altmann, Philipp; Cokoja, Mirza; Kuehn, Fritz E.; Journal of Organometallic Chemistry; vol. 701; (2012); p. 51 – 55;,
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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. 623-12-1, name is 1-Chloro-4-methoxybenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-Chloro-4-methoxybenzene

General procedure: A Schlenk flask was charged with aryl chlorides (0.20 mmol), arylboronic acids (0.30 mmol), N-heterocyclic carbenepalladium(II) complex 3 (2 mol %), KOtBu (2.0 equiv), iPrOH(1 mL) and H2O (1 mL). The mixture was stirred at 80 C for 15 h under N2. After cooling, the reaction mixture was evaporated andthe product was isolated by preparative TLC on silica gel plates. The purified products were identified by 1H NMR spectra and their analytical data are given in Supporting Information.

The synthetic route of 623-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Tao; Xie, Huanping; Liu, Lantao; Zhao, Wen-Xian; Journal of Organometallic Chemistry; vol. 804; (2016); p. 73 – 79;,
Chloride – Wikipedia,
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Application of 118-69-4, These common heterocyclic compound, 118-69-4, name is 2,6-Dichlorotoluene, 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.

5 g of catalyst, as described in examples 3 and 4, was loaded in the reactor along with the diluent corundum particles (1: 1 by weight) and the reaction was performed under the following conditions. A reaction temperature of 350 to [400C] was used, and the GHSV comprised between 650-750 [H-1.] The contact time consisted of 4.8 to 5.5 seconds. The mole ratio of 2,6-DCT : H20 : NH3: air: N2 was 1: 15: 3-4: 21, the molar concentration of 2,6- DCT was 2.4 % and the ratio of [0/NH3] was 1. [1 %.]

The synthetic route of 118-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TESSENDERLO CHEMIE S.A.; WO2003/101939; (2003); A2;,
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 6775-78-6 as follows. Formula: C6H4ClN3

478 mg (3.11 mmol) of 6-chloroimidazo[1 ,2-b]pyridazine were introduced into 10 mL of chloroform under argon and, while cooling in ice, 664 mg (3.73 mmol) of N-bromosuccuinimide were added. After the addition was complete, the reaction mixture was stirred at rt over night. The reaction mixture was then mixed with water and ethyl acetate and, after addition of saturated sodium bicarbonate solution, the phases were separated. The aqueous phase was extracted three more times with ethyl acetate. The combined organic phases were then washed with sat. sodium chloride solution and dried over sodium sulfate. In the final removal of the solvent in vacuo, the desired product was isolated in quantitative yield in the form of an amorphous white solid which was employed without further chromatographic purification in subsequent reactions. 1H-NMR (CDC , stored over molecular sieves): delta [ppm] (1 H) ppm.

According to the analysis of related databases, 6775-78-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bayer Intellectual Property GmbH; EIS, Knut; PUeHLER, Florian; ZORN, Ludwig; SCHOLZ, Arne; LIENAU, Philip; GNOTH, Mark, Jean; BOeMER, Ulf; GUeNTHER, Judith; HITCHCOCK, Marion; WO2013/34570; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics