Month: May 2021

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. 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 18282-59-2

A solution of 1-bromo-3,4-dichlorobenzene (16.92 g, 0.074 mol) in Et2O (100 ml) was added to a suspension of magnesium turnings in Et2O (60 ml) and the mixture was refluxed for 1 hour. The reaction was cooled to 23¡ã C. and a solution of 4-cyanopyridine 54 (7.80 g, 0.075 mol) in 1:1 Et2O:THF (150 ml) was added rapidly with vigorous stirring. The mixture was refluxed for 24 h, then cooled to 23¡ã C. Ice (100 g) was added, followed by 50percent H2SO4 (50 ml), and the mixture was stirred for 1 h. Et2O (100 ml) was added, the aqueous layer was separated, made basic with 10percent NaOH, and extracted with EtOAc (2.x.250 ml). The combined organic layer was dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography (eluant: 30percent EtOAc: CH2Cl2) gave 12 g (0.047 mol, 64percent) of the product 55 as a colorless oil. MS (FAB for M+1): m/e 252.

According to the analysis of related databases, 18282-59-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SCHERING CORPORATION; US2005/182095; (2005); A1;,
Chloride – Wikipedia,
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Application of 2613-30-1, 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. 2613-30-1, name is 4-Chloro-2,5-difluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2. Preparation of 1-Bromo-4-chloro-2,5-difluorobenzene Anhydrous copper (II) bromide (2.7 g, 12.1 mmol) and t-butyl nitrite (1.56 g, 15.1 mmol) were combined in anhydrous acetonitrile (25 mL). The resulting mixture was heated to 65 C. and a solution of 4-chloro-2,5-difluoro-phenylamine (1.65 g, 10.1 mmol) in anhydrous acetonitrile (2 mL) was added dropwise (vigorous gas evolution was noted). After the reaction mixture cooled ambient temperature, it was added to 2N HCl and extracted with ether twice. The organic extracts were then combined, washed with 2N HCl, washed with saturated sodium bicarbonate, dried, concentrated and purified by flash chromatography on silica gel (hexanes) to give the title compound as a white solid (1.11 g, 48.4% yield): 1H NMR (CDCl3): delta 7.38 (dd, 2H), 7.21 (dd, 2H).

The synthetic route of 4-Chloro-2,5-difluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Epp, Jeffrey B.; Schmitzer, Paul R.; Guenthenspberger, Katherine A.; Lo, William C.; Siddall, Thomas L.; US2009/62125; (2009); 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. 771583-81-4, name is 4-Chloro-2-(trifluoromethyl)benzylamine, A new synthetic method of this compound is introduced below., Formula: C8H7ClF3N

5-((4- (ethylsulfonyl) benzyl) carbamoyl) -2- (2-fluoroethoxy) benzoic acid (200.0 mg, 0.5 mmol), HATU (278.6 mg, 0.7 mmol) and DIPEA (189.0 mg, 1.5 mmol) was dissolved in tetrahydrofuran (10 mL), and after stirring at room temperature for 0.5 hours, 4-chloro-2- (trifluoromethyl) benzylamine (153.6 mg, 0.7 mmol) was added. At room temperature After reacting for 4 hours, an appropriate amount of water was added and extraction was performed 3 times with ethyl acetate. The organic phases were combined and washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated. The concentrate was purified by preparative high performance liquid chromatography to obtain the title compound (150.0 mg, yield: 51%) in this step.

The synthetic route of 771583-81-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Kelun Botai Bio-pharmaceutical Co., Ltd.; Liu Chunchi; Liu Jinming; Ren Yun; Cai Jiaqiang; Wang Lichun; Wang Jingyi; (42 pag.)CN110724075; (2020); A;,
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Electric Literature of 626-43-7,Some common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, molecular formula is C6H5Cl2N, 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: The syntheses of the ferrocenyl phenylguanidines were achieved in four steps (Scheme-1 suppl). In the first step; nitrophenylferrocene (a and b) were made by the coupling of ferrocene with diazonium salts of nitroaniline using phase transfer catalyst [20]. In the second step; these nitro phenyl ferrocene were reduced into ferrocenylaniline (c and d) using palladium on charcoal and hydrazine as reducing agent [21]. In the third step three different chloro-substituted thioureas (e) were synthesized by the coupling of substituted aniline with thiocynates in acetone [22]. In the fourth step; the benzoylphenylthiourea (e) were mixed with the ferrocenyl aniline (c and d) in dimethyl formamide (DMF) in equimolar ratio with two equivalents of triethylamine (Et3N). The temperature was maintained below 5C using an ice bath and one equivalent of mercuric chloride (HgCl2) was added to the reaction mixture with vigorous stirring. The ice bath was removed after 30min while the stirring continued overnight. The progress of the reaction was monitored by thin layer chromatography (TLC) till the completion of reaction. Chloroform (CHCl3, 20ml) was added to the reaction mixture and the suspension was filtered through a sintered glass funnel to remove the mercuric sulfide (HgS) residue. The solvents from filtrate were evaporated under reduced pressure and residue was re-dissolved in dichloromethane (CH2Cl2, 20ml), washed with water (4¡Á30ml) and dried the organic phase over anhydrous magnesium sulfate (MgSO4). The solvent was evaporated and residue was purified by column chromatography to afford ferrocenyl phenylguanidines (f and g) [23]. Solid and liquid state characterization data is given in Supplemental part

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

Reference:
Article; Gul, Rukhsana; Badshah, Amin; Khan, Azim; Junaid, Asif; Rauf, Muhammad Khawar; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 117; (2014); p. 264 – 269;,
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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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 14752-66-0

(b) Sodium 4-chlorophenylsulfi nate [9.93 g(0.05 mol)] and monochloroacetic acid [4.72 g(0.05 mol)] were dissolved in 20 mL of water, adjustedto pH 10 with a NaOH solution, and boiled in a waterbath for 1 h. The reaction mixture was cooled, and extractedwith benzene (2 ¡Á 30 mL). From the benzenesolution, after distilling off the solvent, 0.67 g (7%)of sulfone (3), i.e., 4-lC6H4SO2CH3 was obtained,mp 93-95C. Found, %: 44.30, 3.58, Cl 18.41,S 16.67. 77Cl2S. Calculated (%): 44.10, 3.71,Cl 18.59, S 16.82The aqueous layer was acidifi ed with HCl untilneutral and held at 5C for 12 h. The precipitate wasrecrystallized (chloroform-hexane, 1 : 2) and dried invacuo over P2O5. 10.78 g (92%) of acid (1) was obtained,mp 120-122C.

According to the analysis of related databases, 14752-66-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Adamovich; Oborina; Mirskova; Russian Journal of Applied Chemistry; vol. 91; 4; (2018); p. 701 – 705; Zh. Prikl. Khim. (S.-Peterburg, Russ. Fed.); vol. 91; (2018); p. 602 – 606,5;,
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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. 95-49-8, name is 1-Chloro-2-methylbenzene, A new synthetic method of this compound is introduced below., name: 1-Chloro-2-methylbenzene

In a 250 mL four-necked flask was added 141 mL (150 g) o-chlorotoluene, adding 3.0 g Hbeta molecular sieve catalyst, stirring to disperse evenly; and then into the system by 50 mL / min sulfuric acid dry chlorine gas, at 35 C for 12 h to give dichlorotoluene. After the exhaust gas is condensed, the unreacted Cl2 is removed by the NaOH solution.

The synthetic route of 95-49-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing Zhongteng Chemical Co., Ltd.; Zhong Hua; Lu Minshan; Chen Xiuzhen; Liu Qiaobao; Yin Hengbo; Wang Aili; (8 pag.)CN104876790; (2017); B;,
Chloride – Wikipedia,
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Related Products of 50638-46-5, The chemical industry reduces the impact on the environment during synthesis 50638-46-5, name is 4-Bromo-3-chloroanisole, I believe this compound will play a more active role in future production and life.

Step C: Preparation of a-(2-chloro-4-methoxyphenyl)- 1 -(2,6-difluorophenyl)- 1H- imidazole-5 -methanol; To a mixture of l-bromo-2-chloro-4-methoxybenzene (5.31 g, 24.0 mmol) in tetrahydrofuran (40 mL) cooled in an ice-water bath was added dropwise isopropylmagnesium chloride lithium chloride complex (1.3 M tetrahydrofuran, 18.4 mL, 24.0 mmol) over 15 minutes. The reaction mixture was allowed to warm to ambient temperature (about 20 C) and stirred for 16 h. After 16 h, the reaction mixture was cooled to 0 C and l-(2,6-difluorophenyl)-lH-imidazole-5-carboxaldehyde (i.e. the product of Step B) (2.50 g, 12.0 mmol) in tetrahydrofuran (10 mL) was added dropwise. The reaction mixture was stirred for about 15 minutes, and then saturated aqueous ammonium chloride solution (about 3 mL) was added. After about 5 minutes more saturated aqueous ammonium chloride solution (about 100 mL) was added and the resulting mixture was extracted with ethyl acetate (100 mL). The organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered and concentrated under reduced pressure to provide the title compound as a white solid (2.77 g).in NMR (CDCI3): delta 7.51 (s, 1H), 7.43 (m, 1H), 7.38 (d, 1H) 7.1-7.0 (m, 2H), 6.9 (m, 1H), 6.82 (m, 1H), 6.78 (m, 1H), 5.98 (m, 1H), 3.80 (s, 3H), 2.4 (m, 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, 4-Bromo-3-chloroanisole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; LONG, Jeffrey, Keith; BEREZNAK, James, Francis; KAR, Moumita; TAGGI, Andrew, Edmund; CHEN, Yuzhong; WO2012/44650; (2012); A1;,
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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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-(Chloromethyl)benzo[d][1,3]dioxole

To a slurry of magnesium turnings (1.09 g, 44.8 mmol) in 5 mL of THF was added iodine (0.0650 g, 0.256 mmol), followed by a solution of 5-(chloromethyl)benzo[d][l,3]dioxole. (6.55 g, 38.4 mmol) in 30 mL of THF. After 1 minute, the exothermic reaction mixture was placed in an ice bath for 1 minute and then stirred at ambient temperature for 1 hour. TMEDA (7.68 ml, 51.2 mmol) was added to the reaction and the mixture was cooled to -78 0C for 5 minutes at which point a solution of (E)-N-((S)-2,3-bis(tert- butyldimethylsilyloxy)propylidene)-2-methylpropane-2-sulfinamide (5400 mg, 12.8 mmol) in 25 mL THF was added via a syring pump over 15 minutes. The reaction was allowed to warm to RT over the course of 2 hours then stirerd at RT for an additional hour. The mixture was diluted with ethyl acetate (10O mL) and poured in saturated ammonium chloride (250 mL). The aqueous layer was extracted with ethyl acetate (2 x 250 mL) and the combined organic layers were washed with water and then brine and dried over Na2Stheta4. The organic colvents were filtered, concentrated under reduced pressure and the crude material was purified by silica gel to provide N-((2R,3 S)-I- (benzo[d][l,3]dioxol-5-yl)-3,4-bis(tert-butyldimethylsilyloxy)butan-2-yl)-2- methylpropane-2-sulfinamide (4.51 g, 63.1% yield) as a colorless oil.

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AMGEN INC.; WO2008/147547; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 61881-19-4,Some common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, molecular formula is C8H5ClF3N, 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: Add sodium acetate, trifluoroethylimidyl chloride (II), hydrazone (III), and 1 mL of organic solvent to the 35 mL Schlenk tube according to the raw material ratio in Table 1.Mix and stir well. After the reaction is completed according to the reaction conditions in Table 2, 2-4 hours,Add elemental iodine, continue the reaction for 1-2 hours, filter, and stir the sample in silica gel.After purification by column chromatography, the corresponding 5-trifluoromethyl-substituted 1,2,4-triazole compound (I) is obtained. The reaction process is shown by the following formula:

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, its application will become more common.

Reference:
Patent; Zhejiang Sci-Tech University; Chen Zhengkai; Hu Sipei; Yang Zuguang; (10 pag.)CN110467579; (2019); A;,
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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, A new synthetic method of this compound is introduced below., Quality Control of 3-Chloro-2-chloromethyl-1-propene

Sodium hydride (60% in mineral oil) (0.99 g, 24.81 mmol) was dissolved in DMF (20 mL) at 0 C and 3-chloro-2-(chloromethyl)prop-1-ene (1.31 mL, 12.41 mmol) was added in portions. Separately N-boc-ethanolamine (1.92 mL, 12.41 mmol) was dissolved in THF (20 mL) and added dropwise. The reaction mixture was stirried at 20 C for 21 h. The volatiles were removed under reduced pressure. The reaction was diluted with water (50 mL) and then extracted with EtOAc (3 x 80 mL). The organic extracts were combined passed through a phase separation cartridge and the volatiles were removed under reduced pressure. The crude product was dissolved in DCM and purified via silica gel chromatography eluting with 0-50% EtOAc in heptane to afford tert-butyl 6-methylene-1,4-oxazepane-4-carboxylate (1.25 g, 47%) as a clear oil. 1H NMR (400 MHz, CDCl3) 1.46 (s, 9H), 3.37 – 3.45 (m, 2H), 3.64 – 3.79 (m, 2H), 4.00 – 4.24 (m, 4H), 4.88 – 5.04 (m, 2H); 13C NMR (400 MHz, DMSO, 100 C) 28.58, 50.40, 51.72, 71.82, 74.29, 79.44, 112.06, 146.96, 154.80; HRMS [M+H]+ measured 236.1274, C11H19NO3 requires 236.1263.

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; Watson, David W.; Gill, Matthew; Kemmitt, Paul; Lamont, Scott G.; Popescu, Mihai V.; Simpson, Iain; Tetrahedron Letters; vol. 59; 51; (2018); p. 4479 – 4482;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics