Author: Jessica.F

6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, 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. SDS of cas: 6579-54-0

Taking 245 mg 2,6-dichlorobenzenesulfonyl chloride dissolved into 20 ml anhydrous methanol, stirring 20 min, add m-phenylenediamine 450 mg and triethylamine 3 ml, in 70 C under stirring 12 h cooling, methanol, water, extracted with ethyl acetate three times, the combined organic phase, water washing, water-free MgSO4Drying, evaporating the solvent, purification with silica gel column chromatography, eluting agent volume ratio: AcOEt: petroleum ether=1:4, to obtain white solid N,N’-bis(2,6-dichlorobenzenesulfonyl)m-phenylenediamine 515 mg, yield 98%.

The synthetic route of 6579-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jishou University; Xiao Zhuping; Ni Weiwei; Fu Zijuan; Yi Juan; Zhou Tianli; (21 pag.)CN109096156; (2018); A;,
Chloride – Wikipedia,
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118-69-4, name is 2,6-Dichlorotoluene, 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. Safety of 2,6-Dichlorotoluene

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

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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Chloro-N,N-dimethylethanamine hydrochloride

A mixture of the 4-hydroxybenzaldehyde (100g, 0.82mol) and anhydrous K2CO3 (330g,2.5mol) in EtOAc (1000mL) was stirring at 80 C till the disappearance of the startingmaterials 4-hydroxybenzaldehyde. Then 2-chloro-N, N-dimethylethanaminehydrochloride (118.69g, 0.83mol) was added into the reaction system and continued tostir until the reaction finished. After reaction, the mixture was filtered and the filtratewas washed with water and dried with Na2SO4. The extraction was filtered and thefiltrate was evaporated under reduced pressure to recycle the ethyl acetate and give thecrude mass which was further evaporated under high vacuum (bp142 -144oC/0.533 kPa)to give pale yellow oil(181.42g, 94%).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Feng, Chengliang; Yan, Bin; Yin, Guibo; Chen, Junqing; Ji, Min; Synlett; vol. 29; 17; (2018); p. 2257 – 2264;,
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Synthetic Route of 873-38-1, These common heterocyclic compound, 873-38-1, name is 2-Bromo-4-chloroaniline, 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.

To a well-stirred mixture consisting of 2-bromo-4-chloroaniline (5.0 g, 24 mmol) in tetrahydrofuran (180 ML), diethyl-3-pyridyl borane (4.07 g, 28 MMOL), and bis (TRIPHENYLPHOSOPHINE) PALLADIUM (II) chloride (2.53 g, 3.6 mmol), a solution of sodium carbonate (12.72 g, 120 MMOL) in water (60 ML) was added. The reaction was then heated at 75C for 18 hours. The layers of the biphasic mixture were separated, and the aqueous phase was extracted with an equal volume of ethyl acetate. The combined original reaction organic phase and ethyl acetate extract were dried and concentrated in vacuo to afford an oil (9.4 g). Flash chromatography of the entire sample (silica gel ; initial elution with ethyl acetate/hexanes = 8: 2 in volume followed by elution with pure hexane) afforded the title compound as a colorless oil (3.64 g, 74% yield). TLC Rf (silica gel plates ; elution with ethyl acetate, UV detection): 0.46.

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

Reference:
Patent; PFIZER PRODUCTS INC.; WO2004/43929; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 210532-25-5, 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. 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 2; N-r5-( 4-Amino-7 -isopropvl-7 H-pvrrolor2 .3-dl pvrim idine-5-carbonvl)-pvrid in-3-vll-3,5- difluoro-benzenesulfonamide; 3,5-Difluoro-benzenesulfonyl chloride (19.7 mg, 0.093 mmol) was added to a solution of (4-Amino-7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(5-amino-pyridin-3-yl)-methanone (25 mg, 0.084 mmol) in pyridine (0.7 mL). The resulting solution was heated to 40 C for 16 h. The reaction mixture was concentrated in vacuo and the residue dissolved in DMSO (2 mL) and purified using reverse phase preparative HPLC to furnish the title compound as a white solid. MS: 473.2 (MH+) ; HPLC Rf: 4.91 min. (HPLC method 4).

The synthetic route of 3,5-Difluorobenzene-1-sulfonyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2005/116035; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 13726-14-2, name is 4-Chloro-3-methoxyaniline, 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 13726-14-2, Recommanded Product: 4-Chloro-3-methoxyaniline

5-NITRO-2-CHLORO aniline (50.0 g, 0.289 mol) in 30 % sulfuric acid (300 ml) was stirred at RT FOR 2 h. Sodium nitrite (21.0 g, 0.304 mol) in water (50 ml) was added slowly at 0C and maintained at this temperature for 15 min. This diazotized solution was added slowly to dilute sulfuric acid (50 %, 250 ML) at 110 C. Stirring was continued for 15 min. After cooling to RT, ice water was added, the mixture extracted with ethylacetate, washed with water, brine and dried over NA2SO4. The product obtained upon concentration was purified by column chromatography. Yield 12.0 g, 24. 0 %. [00162] To K2CO3 (23.84 g, 0.172 mol) and 2-chloro-5-nitrophenol (10.0 g, 0.0576 mol) in ACETONITRILE (100 ml) was added methyl iodide (19.60 g, 0.138 mol) at 0C. The reaction mixture was warmed to RT and stirred overnight. Water was added and extracted with ethyl acetate. The organic layer was washed with water, brine and dried over NA2SO4. The product obtained upon concentration was purified by column chromatography. Yield : 6.0 g, 55. 55 %. [00163] 2-CHLORO-5-NITRO ANISOLE (6.0 g, 0.032 mol) in MEOH (45 ml) was added slowly to stannous chloride (15.1 g, 0.08 mol) in conc. HCI (110 ml) at 40 C and the temperature was slowly raised to 50 C. Stirring was continued for 2h, the reaction cooled to RT, basified with 50 % NAOH solution and extracted by ethyl acetate. The organic layer was washed with water, brine and dried over NA2SO4. The product obtained upon concentration was purified by column chromatography. Yield : 4.0 g, 79.36 %. [00164] To triethylamine (3.83 g, 0.037 mol) and 3-methoxy-4- chloro aniline (3.0 g, 0.0190 mol) in benzene (50 ML) was added trimethylacetylchloride (2.75 g, 0.022 mol) slowly at 0 C. The temperature was raised to RT and stirred overnight. The reaction mixture was added to ice and extracted with ethyl acetate. The organic layer was washed with water, brine, dried over NA2SO4 and concentrated. Yield : 3.7 g, 80.43 %. [00165] To N-PIVALOYL-3-METHOXY-4-CHLOROANILINE (1.50 g, 0.0062 mol) in THF (30 ML) was added n-butyl lithium (1.0 g, 0.0156 mol) at 0 C and the reaction stirred for 2 hr. After cooling to-70 C, methyl isonicotinate (1.3 g, 0.0094 mol) in THF (12 ml) was added slowly. The reaction was warmed to rt and stirred overnight and then quenched with water and extracted with ether. The water layer was further extracted and the combined ether layers were washed with water, brine and dried over NA2SO4. The product obtained upon concentration was purified by column chromatography. Yield 0.50 g, 23. 25 %. [00166] The protected ketone from step 5 (0.500g, 0. 0014MOL) was suspended in concentrated HCI (5 ml) at RT, then the temperature was raised to 95 C and the mixture stirred over night. The mixture was cooled to RT, basified with 20 % NAOH solution and extracted with DCM. The combined organic layer was washed with water, brine and dried over NA2SO4. The product obtained upon concentration was purified by column chromatography using basic alumina to yield title compound (0.140 g, 37.33%).

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-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CHEMOCENTRYX; WO2004/46092; (2004); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 22680-44-0, name is (2-Chlorophenyl)methanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., category: chlorides-buliding-blocks

45-1) 5-Hydroxymethyl-1-(2-chlorobenzyl)imidazole The title compound was obtained in a yield of 60% according to the same procedure as Preparation 31-1) using dihydroxyacetone and 2-chlorobenzylamine hydrochloride as sting materials. 1H NMR(CDCl3) delta3.24(s, 2H), 4.44(s, 2H), 5.26(s, 2H), 6.78(d, 1H), 6.90(s, 1H), 7.15(m, 1H), 7.21(m, 1H), 7.34(d, 1H), 7.38(s, 1H)

According to the analysis of related databases, 22680-44-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LG Chemical Ltd.; US6268363; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 7149-75-9, 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. 7149-75-9, name is 4-Chloro-3-methylaniline, This compound has unique chemical properties. The synthetic route is as follows.

Synthesized according to General Procedure 1. 4-chloro-3-methylaniline (5 g, 35.3 mmol) in water (15 mL) and conc. HCl (9.5 mL, 116.5 mmol) at -5¡ã C. was added a freshly prepared aqueous solution of sodium nitrite (3.2 g, 45.9 mmol) in water (8 mL) slowly over 10 minutes. After stirring for 15 minutes at -5¡ã C. a freshly prepared aqueous solution of sodium tetrafluoroborate (5.4 g, 49.4 mmol) in water (14 mL) was added in one portion causing the formation of a precipitate. The solid was filtered and washed with cold (5¡ã C.) diethyl ether (10 mL). The solid was dissolved in acetone (15 mL) and filtered. To the filtrate was added diethyl ether (15 mL) causing the precipitation of the arenediazonium tetrafluoroborate. The solid was filtered, washed with cold (5¡ã C.) diethyl ether (5 mL) and then air dried overnight to provide 4-chloro-3-methylbenzenediazonium tetrafluoroborate (8.07 g, 33.6 mmol, 95percent yield) as a tan solid. 1H-NMR (400 MHz, DMSO-d6) delta 8.68 (d, J=2.2 Hz, 1H), 8.56 (dd, J=2.4, 8.8 Hz, 1H), 8.10 (d, J=8.8 Hz, 1H) and 3.47 (s, 3H) ppm. LC/MS (10percent-99percent CH3CN (0.035percent TFA)/H2O (0.05percent TFA), m/z: M+1 obs=125.0; tR=0.24 min.

The chemical industry reduces the impact on the environment during synthesis 4-Chloro-3-methylaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; US2010/4300; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 174913-12-3, A common heterocyclic compound, 174913-12-3, name is 1-Bromo-3-chloro-5-methoxybenzene, molecular formula is C7H6BrClO, 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.

Bromo-3-chloro-5-methoxybenzene (10 mmol, 2.2 g)Diphenylamine (20 mmol, 3.34 g) was added to a 100 mL three-necked flask,A cuprous iodide (2 mmol, 0.4 g) was added under nitrogen,Potassium carbonate (20 mmol, 1.4 g),O-phenanthroline (2 mmol, 0.4 g),50 mL of DMF,Reaction was carried out at 155 C for 3 days;The resulting reaction product is subjected to extraction,The extracted organic phase was evaporated to dryness with ethanol,Then recrystallized from ethyl acetate and petroleum ether,To obtain 1.83 g of intermediate A-1,

The synthetic route of 174913-12-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jilin Aolai De Optoelectronic Materials Co., Ltd.; Gao, Chunji; Cui, Dunzhu; Sun, Yi; Zhang, Chengcheng; (52 pag.)CN104892434; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2106-04-9, A common heterocyclic compound, 2106-04-9, name is 3-Chloro-2-fluoroaniline, molecular formula is C6H5ClFN, 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.

Step 1: 5-Bromo-N-(3-chloro-2-fluorophenyl)pyridin-3-amineA 20 mL microwave vial was charged with 3-chloro-2-fluoroaniline (473 jiL, 4.22 mmol) and diluted with 1,4-dioxane (16.9 mL). To that solution was added 3,5- dibromopyridine (1000 mg, 4.22 mmol), sodium tert-butoxide (568 mg, 5.91 mmol),xantphos (48.9 mg, 0.0840 mmol), and tris(dibenzylideneacetone)dipalladium(0) (38.7 mg, 0.0420 mmol). The vial was sealed and degassed using ultra pure argon and sonication for 1 mm. The vial was placed into a reaction block preheated to 80 C. After 1 h, the contents of the vial were transferred to a flask, and the volatiles were concentrated under reduced pressure. The resulting brown solids were dissolved with ethyl acetate andwater. The contents of the flask were transferred into a separatory funnel where the layers were separated. The organic was washed with water and brine, dried over magnesium sulfate, and purified by silica gel flash chromatography. Upon dissolving the sample with DCM, a white solid persisted, which was collected by filtration and washed with hexanes to give 541 mg of desired product. The supernatant was concentrated under reducedpressure and purified by silica gel column chromatography (24 g ISCO RediSep Rf, loaded inlwith: DCM and dried, initial waste: 0 mL, fraction size: 9 mL 13x 100 mm, and eluted with ethyl acetate in dichloromethane 0% [75 mL], 0-5% [201 mL], 5% [300 mL]).The fractions were collected and combined with the previously collected solids to give 921 mg(72%). ?H NMR (400MHz, CDC13)oe 8.35 (d,J=2.5 Hz, 1H), 8.31 (d,J1.8 Hz, 1H), 7.58 (t,J=2.1 Hz, 1H), 7.22-7.14 (m, 1H), 7.08-7.01 (m, 2H), 5.86 (br. s., 1H). Mass found 302 [M+H] .

The synthetic route of 2106-04-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; NORRIS, Derek J.; DELUCCA, George V.; GAVAI, Ashvinikumar V.; QUESNELLE, Claude A.; GILL, Patrice; O’MALLEY, Daniel; VACCARO, Wayne; LEE, Francis Y.; DEBENEDETTO, Mikkel V.; DEGNAN, Andrew P.; FANG, Haiquan; HILL, Matthew D.; HUANG, Hong; SCHMITZ, William D.; STARRETT, JR, John E.; HAN, Wen-Ching; TOKARSKI, John S.; MANDAL, Sunil Kumar; WO2015/100282; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics