Month: May 2021

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. 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, A new synthetic method of this compound is introduced below., Recommanded Product: 3,6-Dichloro-1,2,4,5-tetrazine

General procedure: To a solution of DIPEA (2.1 mmol) in acetonitrile (150 mL) which was preheated to 70 C was added dropwise a solution of 3,6-dihydroxyphthalimide derivatives 1a-e (1 mmol) and 3,6-dichlorotetrazine (2, 1 mmol) in acetonitrile (25 mL) during 25 min. After being stirred for another 5 min, the reaction was quenched by cooling down the mixture to ambient temperature and adding water (200 mL). The resulting mixture was neutralized with dilute hydrochloric acid (1 M) and extracted with EtOAc (3 × 150 mL). The combined organic solution was washed with brine (3 × 200 mL) and then dried over anhydrous Na2SO4. After filtration and concentration, the residue was chromatographed on a silica gel column using a mixture of DCM and EtOAc (v/v = 100:1) as an eluent to give product 3a-e.

The synthetic route of 106131-61-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gu, Meng-Di; Lu, Yao; Wang, Mei-Xiang; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 1976 – 1983;,
Chloride – Wikipedia,
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Related Products of 95-81-8, 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. 95-81-8, name is 2-Chloro-5-methylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 2A 10.0 g (70.6 mmol) of 2-chloro-5-methyl-aniline were dissolved in 38 ml hydrochloric acid (20% in water). At -5C a solution of 5.36 g (77.7 mmol) of sodium nitrite in 70 ml water was added drop wise within 40 min and kept at this temperature for further 30 min. The cold solution was added drop wise to a solution of 40.2 g (178 mmol) of tin(ll)-chlohde dihydrate in 48 ml of hydrochloric acid (32% in water), maintaining the temperature at -100C. The resulting suspension was heated to 25C and stirred for 12 h. The suspension was cooled to 00C and 350 ml sodium hydroxide (40% in water) were added. The solution was extracted with ethyl acetate three times. The organic layers were collected, extracted with water and dried over magnesium sulphate. Filtration and evaporation of the solvent under reduced pressure yielded the hydrazine as a solid. (9.6 g, 87% of theory).HPLC-MS (Method 1 ): RT: 0.90 minMS (ESI pos): m/z = 157/159 (Cl) (M+H)+ and 140/142 (Cl) (M-NH3+H)+.

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-Chloro-5-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WO2009/68617; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 38762-41-3, A common heterocyclic compound, 38762-41-3, name is 4-Bromo-2-chloroaniline, molecular formula is C6H5BrClN, 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: Experimental Procedure: A dried 25 mL Schlenk tube equipped with a magnetic stir bar was charged with Togni?s Reagent 2 (0.25 mmol, 1.0 equiv), free anilines 1 (0.75 mmol, 3.0 equiv), K2CO3 (0.375 mmol, 1.5 equiv) and CH3CN (1.5 mL). The reaction mixture was then stirred at 75 C for 6 h under an argon atmosphere. The reaction progress was monitored by TLC. After cooling to room temperature, the mixture was washed with water and extracted with CH2Cl2 three times, then washed with saturated NaCl solution. The combined organic layer was dried with anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo. The crude product was purified by flash column chromatography on silica gel (Elutent: petroleum ether-EtOAc) to give the pure product. The products were characterized by 1H NMR, 13C NMR, 19F NMR, GC -MS.

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

Reference:
Article; Chen, Xiaoyu; Ding, Licheng; Li, Linlin; Li, Jingya; Zou, Dapeng; Wu, Yangjie; Wu, Yusheng; Tetrahedron Letters; vol. 61; 9; (2020);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 328-84-7, 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. 328-84-7, name is 3,4-Dichlorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

a. 1,3-Bis(2-chloro-alpha,alpha,alpha-trifluoro-p-tolyloxy)benzene A solution of potassium hydroxide (3.26 g. 0.05 mole, 85%) in water (~3 g.) is added slowly dropwise to a solution of resorcinol (2.75 g. 0.025 mole) and 3,4-dichloro-alpha,alpha,alpha-trifluorotoluene (10.75 g. 0.05 mole) in sulfolane (125 ml) at 150-160 C., with stirring. When the addition is complete, the strongly colored reaction mixture is stirred at 150-160 C. overnight, then cooled, diluted with benzene (200 ml), and washed cautiously with water (700 ml). Hexane (200 ml) is added and the mixture washed with water (600 ml), dilute sulfuric acid (600 ml), dilute sodium hydroxide solution (600 ml), and water (600 ml), dried, and the solvent removed to give 1,3-bis(2-chloro-alpha,alpha,alpha-trifluoro-p-tolyloxy)benzene (8.6 g. 65%) b.p. 160-70 C./0.1 mm.

The synthetic route of 3,4-Dichlorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rohm and Haas Company; US31455; (1983); E1;; ; Patent; Rohm and Haas Company; US4063929; (1977); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 7149-75-9, 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. 7149-75-9, name is 4-Chloro-3-methylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 4-chloro-3-methylaniline (0.500 g, 3.53 1 mmol) and pyridine (0.427 mL, 5.297 mmol) in dichloromethane (20 mL) was mixed at the room temperature with ethanesulfonyl chloride (0.400 mL, 4.237 mmol) and stuffed at the same temperature for 12 hr. Then, aqueous 1M-hydrochloric acid solution was added to the reaction mixture, followed by extraction with dichloromethane. The bi-phasic mixture was passed through a plastic frit to remove the solid residues and aqueous layer, and the organic layer collected was concentrated in vacuo. The residue was chromatographed (Si02, 12 g cartridge; ethyl acetate / hexane = 5 percent to 50 percent) to give N(4-chloro-3-methylphenyl)ethanesulfonamide as beige solid (0.440 g, 53.3 percent).

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-Chloro-3-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CHONG KUN DANG PHARMACEUTICAL CORP.; LEE, Jaekwang; HAN, Younghue; KIM, Yuntae; CHOI, Daekyu; MIN, Jaeki; BAE, Miseon; YANG, Hyunmo; KIM, Dohoon; (644 pag.)WO2017/18803; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 112-26-5, 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. 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In a 50 mL round bottom flask imidazole (32 mmol, 2.176 g) and potassium hydroxide (32 mmol, 1.792 g) were dissolved in DMSO (25 mL). The mixture was stirred at 70 for 1 h. After this time, 1,1?-oxybis(2-chloro-ethan (16 mmol, 1.88 ml) was added into the solution and stirred for 24 h under nitrogen atomosphere to complete the reaction which was monitored by TLC. The resulting mixture was poured into 100 mL of water and extracted with methylene chloride (5×20 mL). The combined organic layer was washed with water (3×20mL), dried over Na2SO4 and concentrated to give the crude product, which was further purified by column chromatography over silica gel using CH2Cl2 as eluent to give 1a as a pale yellow viscous oil (2.04 g, Yield = 62% ).

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, 1,2-Bis(2-chloroethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhou, Ji; Yuan, Yao-Feng; Zhuo, Ji-Bin; Lin, Cai-Xia; Tetrahedron Letters; vol. 59; 11; (2018); p. 1059 – 1064;,
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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, A new synthetic method of this compound is introduced below., Formula: C8H17Cl2N

To a solution of 1,1-bis(4-hydroxyphenyl)cyclohexane (50.0 mg, 0.186 mmol) in DMF (1.86 mL) at 0 °C was added 60percent sodium hydride (dispersion in paraffin liquid, 44.7 mg, 1.12 mmol). The reaction mixture was stirred for 15 min at 50 °C and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (122 mg, 0.616 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 23 h at 50 °C, saturated aqueous ammonium chloride was added at 0 °C. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 9/1) to afford RID-F-S*103 (compound 29) (62.7 mg, 65percent) as an orange oil

The synthetic route of 26487-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 6775-78-6, These common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, 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.

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 room temperature overnight. 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 (CHLOROFORM-d): delta [ppm] = 7.12 (1 H); 7.79 (1 H); 7.90 (1 H).

Statistics shows that 6-Chloroimidazo[1,2-b]pyridazine is playing an increasingly important role. we look forward to future research findings about 6775-78-6.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; EIS, Knut; PUeHLER, Florian; ZORN, Ludwig; SCHULZE, Volker; SUeLZLE, Detlev; LIENAU, Philip; HAeGEBARTH, Andrea; PETERSEN, Kirstin; BOeMER, Ulf; WO2013/144189; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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: C7H7ClFN

To a solution of 3,4-diflorobenzoyl chloride (45 mL, 358 mmol) in acetonitrile (1.43 L) was added solid potassium thiocyanate (KNCS) (38.2 g, 393 mmol). The suspension was stirred to 0 C for 10 min and then the cooling bath was removed. The suspension was stirred at room temperature for an additional 20 min. A solution of 2-chloro-4-fluorobenzylamine (57.1 g, 358 mmol) in acetonitrile (150 mL) was added over 5 minutes. The resulting suspension was stirred at room temperature for 3 hours. The reaction mixture was diluted with water (1.4 L) and stirred for 1 hour. The suspension was filtered, rinsed with water (150 mL) and dried in vacuo at 60 C to afford N-((2-chloro-4-fluorobenzyl)carbamothioyl)-3,4- difluorobenzamide as a yellow solid (98.3 g, 77% yield). 1HNMR (400 MHz, DMSO-d6) delta 11.56 (bs, IH), 11.12 (t, IH, J=5.7Hz), 8.00 (m, IH), 7.79 (m, IH), 7.54 (m, IH), 7.44 (m, 2H), 7.19 (m, IH), 4.85 (d, 2H, J= 5.7 Hz)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 15205-11-5, its application will become more common.

Reference:
Patent; LYCERA CORPORATION; GLICK, Gary D.; HURD, Alexander R.; TAYLOR, Clarke B.; VANHUIS, Chad A.; WO2012/78874; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 2163-00-0, The chemical industry reduces the impact on the environment during synthesis 2163-00-0, name is 1,6-Dichlorohexane, I believe this compound will play a more active role in future production and life.

Example 4; A nitrogen-purged stirred 2 l four-necked flask apparatus with internal thermometer, reflux condenser with bubble counter and pH electrode was initially charged with 136.5 g (0.55 mol) of sodium thiosulphate pentahydrate and 300 g of deionized water. The stirrer was switched on. After the thiosulphate had dissolved, 38.8 g (0.25 mol) of 1,6-dichlorohexane were added. The weakly acidic mixture was adjusted to pH 7.2+/-0.1 with 2.5% sodium hydroxide solution. The reaction vessel was purged once again briefly with nitrogen and the mixture was then boiled at reflux for 9 h, and the pH of the reaction mixture was kept at 7.2+/-0.1 during this time by addition of 2.5% sodium hydroxide solution by means of a metering pump (control by means of pH electrode). After in each case 6 and 8 hours of the reaction, the bubble counter was removed briefly from the reflux condenser. In each case approx. 5 ml of demineralized water were then sprayed with a wash bottle into the reflux condenser from the top in order to flush back into the flask any 1,6-dichlorohexane which has not dripped back. After the reaction time had ended, approx. 15 ml of 2.5% sodium hydroxide solution were used for pH control. After brief cooling, a small sample was taken from the reaction mixture to determine the conversion of 1,6-dichlorohexane by gas chromatography (GC). The GC analysis with internal standard gave a residual content of 1,6-dichlorohexane <10 ppm, which corresponds to a conversion of 1,6-dichlorohexane of >99.9%. The reaction mixture cooled to room temperature was admixed with 21.0 g (0.25 mol) of aqueous formaldehyde solution (36-38%), 21.0 g (0.25 mol) of sodium hydrogencarbonate and 43.3 g of toluene (25 parts by weight based on 100 parts by weight of the theoretically expected yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane). The headspace of the reactor was purged once again briefly with nitrogen. As soon as the hydrogencarbonate had dissolved, the feed of 773.3 g (0.5 mol) of sodium dibenzyldithiocarbamate solution (NaBEC solution) (19.1%) which had a temperature of approx. 22 C. was commenced at an internal reactor temperature of approx. 23 C. During the uniform feeding of the NaBEC solution over 1 h, the internal reactor temperature was kept at approx. 23 C. On completion of feeding, the mixture was stirred at approx. 23 C. for a further 22 h. Immediately before the commencement of the NaBEC feeding, the pH was approx. 8.3. On commencement of the NaBEC feeding, the pH rose very sharply and attained a value of approx. 10.7 at the end of the NaBEC feeding. At the end of the continued stirring time, the pH was likewise approx. 10.7. It was possible to isolate the precipitated solid very readily by suction filtration. The product was washed on the suction filter with a total of 2 1 of demineralized water in portions, which proceeded very easily. The product was dried at 50 C. and approx. 150 mbar in a vacuum drying cabinet to constant weight. The yield was approx. 91% of theory based on 1,6-dichiorohexane used. The content of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was determined to be approx. 96% by means of HPLC (external standard). The melting point was approx. 92 C. The ignition residue (750 C./2 h) of the product was approx. 0.2% by weight.

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, 1,6-Dichlorohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Buding, Hartmuth; Weidenhaupt, Hermann-Josef; Jeske, Winfried; Kleiner, Thomas; US2005/272933; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics