Author: Jessica.F

Adding a certain compound to certain chemical reactions, such as: 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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 4584-46-7, category: chlorides-buliding-blocks

General procedure: In a dried single-neck round bottom flask, 4-hydroxylbenzaldehyde (40 mmol), potassium carbonate (122 mmol) and dry acetone (160 ml) were taken and the contents refluxed for 2 h. The reaction mixture was brought to room temperature and catalytic amount of potassium iodide was added, followed by the gradual addition of appropriate dialkylaminoethyl chloride hydrochloride (45 mmol) dissolved in dry acetone (50 ml) through a pressure-equalizing addition funnel and the reaction mixture was allowed to reflux again. The contents were regularly monitored for reaction progress by TLC using 10% methanol/dichloromethane as the solvent system. The reaction was generally complete in 10-13 h. At this point, reaction mixture was filtered under suction and the solid inorganic salts were washed with acetone (3 ¡Á 60 ml). The solvent was evaporated under reduced pressure and the residue was purified by column chromatography over silica gel (6-8% methanol in dichloromethane, v/v as eluent) to afford the pure aldehydes 4a-f as colorless oils in 49-92% yields. The structures of 4a-f were unambiguously established from the comparison of their spectral data with reported values [13,24,25]. The spectroscopic data of compound 4b which is not reported in literature is being included here.

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Reference:
Article; Yadav, Yogesh; MacLean, Erin D.; Bhattacharyya, Annyt; Parmar, Virinder S.; Balzarini, Jan; Barden, Christopher J.; Too, Catherine K.L.; Jha, Amitabh; European Journal of Medicinal Chemistry; vol. 46; 9; (2011); p. 3858 – 3866;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 32137-20-5, name is 1-Chloro-2-fluoro-4-(trifluoromethyl)benzene, 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 32137-20-5, Computed Properties of C7H3ClF4

(b) Preparation of 3(2-chloro-5-trifluoromethylphenoxy)benzoic acid. 3-Hydroxybenzoic acid (3.45 g) was added to a solution of potassium hydroxide (2.8 g) in methanol. The solution was evaporated under reduced pressure to give a white solid. This was taken up in dry dimethylsulphoxide (25 ml). The resulting solution was stirred and heated at 170 with anhydrous potassium carbonate (1.25 g) and 4-chloro-3-fluorobenzotrifluoride (5 g) for 12 hours. The mixture was then cooled and poured into water, (500 ml). The mixture was extracted with ether and then acidified (HCl). The precipitate which formed was recrystallized from petroleum (b.p. 60-80) to give the required acid (4.5 g) with a melting point of 142-143.

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-Chloro-2-fluoro-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Imperial Chemical Industries PLC; US4738711; (1988); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2415-80-7, name is (2,2-Dichlorocyclopropyl)benzene, 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 2415-80-7, Formula: C9H8Cl2

General procedure: a. To a vigorously stirred solution of 0.01 mol of gem-dichloro(bromo)cyclopropane 1a-1h in 30 mL of absolute THF dropwise at -78C under argon 5.5 mL of a 2 M solution of n-butyllithium in cyclohexane (0.011 mol) was added. The resulting mixture was stirred at -78 for 15 min, purged for 2 h at the same temperature with CO2 dried with H2SO4, and then heated to 0C and diluted with 30 mL of water. The aqueous solution was washed with 20 mL of diethyl ether, brought to pH 3 with HCl, and extracted with methylene chloride (3¡Á30 mL). The extract was dried over Na2SO4, and the solvent was removed by distillation to leave alpha-halocyclopropanecarboxylic acids 4a-4h. The spectral characteristics of the products are consistent with those reported in [1, 9]. The mass spectra of the cis and trans isomers of compound 4b-4d are identical to each other. b. The synthesis of 2-substituted alpha-halocyclopropanecarboxylic acids in the presence of LiCl was performed by the same procedure. Lithium chloride, 0.01 mol (0.424 g), was added to the solution of 0.01 mol of gem-dichloro(bromo)cyclopropane 1 before the addition of butyllithium. c. To a vigorously stirred solution of 0.01 mol (0.785 g) of propyl chloride in 30 mL of absolute THF dropwise at -15C under argon 5.5 mL (0.011 mol) of a 2 solution of n-butyllithium in cyclohexane was added. The reaction mixture was heated to 25 and stirred for an additional 60 min. gem-Dihalocyclopropane 1a-1h, 0.01 mol, was then added, and mixture was stirred for 15 min at -78C, after which 5.5 mL of a 2 solution of n-butyllithium in cyclohexane was added. Further workup was performed as described above.

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, (2,2-Dichlorocyclopropyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zagidullin; Zorin; Zorin; Russian Journal of General Chemistry; vol. 86; 10; (2016); p. 2307 – 2311; Zh. Obshch. Khim.; vol. 86; 10; (2016); p. 1659 – 1663;,
Chloride – Wikipedia,
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Synthetic Route 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

Some common heterocyclic compound, 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, molecular formula is C5H2Cl2N4, 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. Recommanded Product: 33050-38-3

General procedure: Appropriate 6-chloro-[1 ,2,4]triazolo[4,3-b]pyridazine (1 eq) or 6-chloro- [1 ,2,4]triazolo[3,4-a]phtalazine (1 eq), potassium carbonate (3 to 4 eq) and the appropriate phenol, thiophenol (1 to 4 eq, 1 eq is preferentially used when R1 = CI) were dissolved in ?,?-dimethylformamide under nitrogen atmosphere. The reaction mixture was stirred overnight at room temperature or at 100-1 10C, or 5-30 minutes at 100-170C on microwave irradiation. The reaction mixture was diluted with ethyl acetate and washed with brine. The organic layer was dried over Na2S04, filtered and evaporated to dryness. The residue was purified by chromatography on silica gel, precipitated, triturated in the appropriate solvent, or used without further purification to obtain the desired 6-aryl-[1 ,2,4]triazolo[4,3-b]pyridazine, or 6-aryl-[1 ,2,4]triazolo[3,4-a]phtalazine.This protocol was used to prepare the following compounds: Cpd.1 -1 , Cpd.1 -3, Cpd.1 -4, Cpd.1 -7, Cpd.1 -8, Cpd.1 -9, Cpd.1 -10, Cpd.1 -1 1 , Cpd.1 -12, Cpd.1 -13, Cpd.1 -14, Cpd.2-1 , Cpd.2-3, Cpd.2-4 and other compounds of the invention that contain a biphenyloxy, a pyridinylphenyloxy, a thiazolylphenyloxy, or a thiopenylphenyloxy group in the 6-substituted position of the [1 ,2,4]triazolo[4,3-b]pyridazines or 6-substituted position of the [1 ,2,4]triazolo[3,4-a]phthalazine (but further information about conditions and purification are reported in Tables of Example 2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 33050-38-3, its application will become more common.

Reference:
Patent; GENFIT; BOUROTTE, Maryline; DELHOMEL, Jean-Francois; DUBERNET, Mathieu; GOUY, Marie-Helene; WO2013/45519; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1005-56-7, A common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, molecular formula is C7H5ClOS, 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: Phenyl chlorothionoformate (345 mg, 2.0 mmol), amine 2 (4.0 mmol) and water (15 mL) were added successively to a 50 mL round-bottom flask. The reaction mixture was stirred at room temperature for 1 h (monitored by TLC). After the reaction was complete, the solid was filtered off, washed with 10% HCl (2 ¡Á 20 mL) and deionised water(2 ¡Á 20 mL), and dried under vacuum to give the pure thiocarbamates 3. All products are known compounds and were identified by comparison of their physical and spectral data with those reported inthe literature.28

The synthetic route of 1005-56-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Zhengyi; Chen, Yuan; Yin, Yue; Wang, Zhiming; Sun, Xiaoqiang; Journal of Chemical Research; vol. 40; 11; (2016); p. 670 – 673;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

873-38-1, name is 2-Bromo-4-chloroaniline, 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. Application In Synthesis of 2-Bromo-4-chloroaniline

4-chloro-2-bromo-aniline (206 mg, 0.01 mmol) was dissolved in dimethylsulfoxide (20 mL). Under a nitrogen atmosphere, bis(pinacolato)diboron (3.8 g, 15 mmol), potassium acetate (2.5 g, 25.7 mmol) and [1,1?-bis(diphenylphosphino)ferrocene]dichloropalladium (218 mg, 0.3 mmol) were added thereto, and the temperature was raised to 80 C. to allow the reaction to proceed for 24 hours. Water (100 ml) was added to the reaction solution, which was extracted with ethyl acetate (80 ml¡Á2). The organic phases were combined, washed with saturated brine (100 mL), dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel column chromatography (ethyl acetate:petroleum ether=1:100 to 1:30) to give the title compound 4-chloro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (2i) as a white solid (2.0 g, yield 79%). 1H NMR (400 MHz, CDC3) delta 7.54 (s, 1H), 7.19-7.08 (m, 1H), 6.55 (d, 1H), 4.86 (s. 2H), 1.34 (s, 12H). LCMS m/z=254.0 [M+1].

The synthetic route of 873-38-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Haisco Pharmaceutical Co., Ltd.; Wei, Yonggang; QIU, Guanpeng; ZHENG, Suxin; LEI, Bolin; YU, Yan; CHEN, Yashu; (29 pag.)US2017/29423; (2017); A1;,
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 69695-61-0 as follows. Recommanded Product: 69695-61-0

(e) Preparation of 5-Methanesulfonyl-pyridine-2-carboxylic acid (2-chloro-4-trifluoromethoxy- phenyl)-amide 7:2-Chloro-4-trifluoromethoxy-phenylamine (2.0 g, 9.29 mmol) in toluene (50 mL) was added to trimethylaluminum (2.0 M 4.65 mL) then methyl 5-(methylsulfonyl)picolinate 6 (1.0 g, 4.65 mol) was added and the mixture was heated to 80-90C for 2 h. The reaction was cooled down and IN HC1 solution (10 mL) was added to be acidic. Dichloromethane (100 mL) was then added and the organic phase was further washed with water (100 mL) and dried over sodium sulfate. The solvent was removed and the residue was mixed with ether (50 mL) and stirred for 0.5 h. The solid was filtered and dried to give 5-methanesulfonyl-pyridine-2-carboxylic acid (2- chloro-4-trifluoromethoxy-phenyl)-amide 7 as a light yellow solid. Yield: 1.26 g, 65%.1H-NMR (300 Hz, CDCI3) delta (ppm): 10.6 (s, 1H), 9.21 (m, 1H), 8.68 (dd, 1H), 8.52 (dd, 1H), 7.40 (dd, 1H),7.22 (m, 2H), 3.20 (s, 3H).

According to the analysis of related databases, 69695-61-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; OSLO UNIVERSITY HOSPITAL HF; HOLSWORTH, Daniel; WAALER, Jo; MACHON, Ondrej; KRAUSS, Stefan; VORONKOV, Andrey Edward; GOLDING, Louise; WO2012/76898; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 69695-61-0, These common heterocyclic compound, 69695-61-0, name is 2-Chloro-4-(trifluoromethoxy)aniline, 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.

An aqueous solution of 2-chloro-4-(trifluoromethoxy)phenylamine (9.0 g) was cooled at 0C, and concentrated hydrochloric acid (75 mL) was dropped slowly to its solution. The reaction mixture was stirred for 30 minutes, and sodium nitrite (3.73 g) was added to the reaction mixture. The reaction mixture was stirred for 40 minutes. An aqueous mixture solution of copper cyanide (4.65 g) and sodium cyanide (7.08 g) which been cooled off in 0C was added to the reaction mixture, and the reaction mixture stirred at room temperature for an hour. The reaction mixture was poured into 5N aqueous solution of sodium hydroxide which been cooled with ice, and extracted twice with ethyl acetate. The organic layer was washed by a saturated aqueous solution of sodium chloride, and dried with anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (high flash-SI, size 4L (made in Yamazen corporation), n-hexane?ethyl acetate/n-hexane=1/8) to obtain a title compound (7.36 g) having the following physical data. TLC:Rf 0.50 (n-hexane/ethyl acetate=20/1); 1H-NMR(CDCl3): delta 7.18 (m, I H), 7.37 (m, 1 H), 7.72 (d, J=8.6 Hz, 1 H).

The synthetic route of 69695-61-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ONO Pharmaceutical Co., Ltd.; EP2154139; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

10061-02-6, name is trans-1,3-Dichloropropene, 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. Recommanded Product: 10061-02-6

PREPARATION OF DIAZOKETONE (4C)Ester (2a) (4.3 g, 28 mmol) was added to a solution of sodium hydride (60% dispersion in mineral oil, 1.4 g, 36 mmol) in DMF (50 mL) at 0 C. The mixture was stirred for 10 min before the addition of 1,3-dichloro-1-propene (1:1 E,Z-mixture, 92%, 4.1 mL, 42 mmol) and warmed to r.t. After 4 h, the reaction was quenched by addition of sat. NH4Cl solution (20 mL), and the reaction mixture was extracted with Et2O (100 mL*2). The organic phase was washed with brine (50 mL), dried over MgSO4, filtered and concentrated. Purification of the residue by flash column chromatography (hexanes-EtOAc, 3:1) gave methyl ester (4a) (1.8 g, 30%).Rf 0.53 (hexanes-EtOAc, 1:1). 1H NMR (500 MHz, CDCl3): d 6.19 (dt, J=1.2, 13.2 Hz, 1H), 5.94 (dt, J=7.9, 13.3 Hz, 1H), 3.85 (s, 3H), 3.16 and 3.02 (ABq, J=18.2 Hz, 2H), 2.67 2.56 (m, 2H), 2.21 (s, 3H). 13C NMR (125 MHz, CDCl3): d 202.7, 168.6, 125.5, 123.7, 118.2, 54.1, 48.9, 44.6, 38.1, 29.6.

The synthetic route of 10061-02-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SNU R&DB FOUNDATION; US2011/28741; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics