Category: chlorides-buliding-blocks

Synthetic Route of 14752-66-0, The chemical industry reduces the impact on the environment during synthesis 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, I believe this compound will play a more active role in future production and life.

A mixture of 8-fluoro-3-iodoquinoline (750 mg, 2.75 mmol), sodium 4- chlorobenzenesulfinate (1.1 g, 5.5 mmol), copper (I) iodide ( 52 mg, 0.275 mmol) and potassium carbonate (380 mg, 2.75 mmol) was treated with lambda^, lambda^-dimethyl-l,2-ethanediamine (49 mg, 0.55 mmol) and anhydrous dimethylsulphoxide (4 ml). The mixture was stirred at 1000C under argon for 8 hr, and cooled to 200C. The reaction mixture was diluted with water (60 ml) and extracted with ethyl acetate (3 x 40 ml). The organic extracts were combined, washed with water (60 ml) and brine (60 ml), dried over magnesium sulphate, and evaporated to dryness. The residue was dissolved in a 1 :1 mixture of dimethylsulphoxide and acetonitrile and purified by mass-directed auto -preparative chromatography using 10 minute gradients containing water and between 50% and 99% acetonitrile with 0.1% formic acid. Product fractions were collected and evaporated to yield the title compound as a white solid (295 mg,deltaH (CDCl3, 400MHz) 7.51-7.69 (4H, m), 7.79 (IH, d, J = 8 Hz), 7.96-7.99 (2H, m), 8.84 (IH, d, J = 2 Hz), 9.30 (IH, d, J = 2 Hz)Mass spectrum: C15H9ClFNO2S requires 321; found 322 (MH+)

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, Sodium 4-chlorobenzenesulfinate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/116816; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1008361-80-5, A common heterocyclic compound, 1008361-80-5, name is 4-Bromo-3-chlorobenzene-1,2-diamine, molecular formula is C6H6BrClN2, 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 solution of 4-bromo-3-chlorobenzene-l,2-diamine (0.1 g) in DMF (2 mL) at room temperature Iota, Gamma-carbonyldiimidazole (0.110 g) was added. The resulting homogeneous solution was stirred overnight at room temperature and then poured into 20 mL of water. The title compound was isolated by filtration, washed with water containing a few drops of 2 N aq. HC1 and dried under high vacuum.

The synthetic route of 1008361-80-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAL, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; GREENLEE, William; (447 pag.)WO2017/35408; (2017); A1;,
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Related Products of 172921-33-4, 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. 172921-33-4, name is 1-Bromo-4-chloro-2,5-difluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3. Preparation of 2-(4-Chloro-2,5-difluorophenyl)-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane 1-Bromo-4-chloro-2,5-difluorobenzene (1.11 g, 4.9 mmol) was dissolved in tetrahydrofuran (THF; 15 mL) and cooled to -10° C. A 2.0M solution of isopropyl-magnesium chloride (2.7 mL, 5.4 mmol) in THF was added dropwise via a syringe. The reaction mixture was stirred at -10° C. for 1 hour, allowed to warm toward 0° C. for 1 hour, then cooled to -10° C. again. A solution of 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.0 g, 5.4 mmol) in THF (1.0 mL) was then added dropwise and the reaction was allowed to warm to ambient temperature. The reaction mixture was then added to diethyl ether and extracted with 1N sodium hydroxide twice. The aqueous phases were combined, acidified to pH 3 with concentrated HCl, and extracted with dichloromethane twice. The organic phases were combined, dried, filtered and concentrated to give the title compound (0.97 g, 72.3percent yield) that was used without further purification: 1H NMR (CDCl3): delta 7.45 (dd, 1H), 7.09 dd, 1H), 1.36 (s, 12H).

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-Bromo-4-chloro-2,5-difluorobenzene, other downstream synthetic routes, hurry up and to see.

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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Application of 363-51-9, 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. 363-51-9, name is 2-Chloro-6-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 2-chloro-6-fluorobenzenamine (5.0 g, 34 mmol) in chlorobenzene (52 mL) was added carbonothioic dichloride (thiophosgene) (5.1 g, 45 mmol) and DMF (0.27 mL). The reaction mixture was refluxed for 2 h and then concentrated to leave the title compound as a brown oil (6.15 g), which was used in Step C without further purification. ¾ NMR delta 7.18 (m, 2H), 7.07 (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, 2-Chloro-6-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; LONG, Jeffrey, Keith; GREGORY, Vann; GUTTERIDGE, Steven; TAGGI, Andrew, Edmund; BEREZNAK, James, Francis; WO2012/31061; (2012); A2;,
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These common heterocyclic compound, 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, 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. category: chlorides-buliding-blocks

To a solution of 3, 6-dichloro- 1,2,4,5 -tetrazine (2.67 g, 17.7 mmol) in methyl ter/-butyl ether (125 mL) at -25 C under nitrogen was added but-3-yn-l -amine hydrochloride (1.87 g, 17.7 mmol), followed by the addition of N,N-diisopropylethylamine (12.4 mL, 70.7 mmol) and the reaction mixture was stirred at -25 C under nitrogen for 26 h. Silica gel (-5 g) was added to the reaction and all solvents were removed in vacuo. The silica gel mesh was loaded on an ISCO silica gel cartridge (220 g) eluting with 25% (0558) EtOAc/hexanes over 2592 mL to afford the title compound (853.3 mg) as a deep red/orange viscous oil,. NMR (400 MHz, CDCh) delta 6.12 (br s, 1H), 3.80 (q, J=6.3 Hz, 2H), 2.63 (td, J=6.3, 2.6 Hz, 2H), 2.10 (t, J=2.6 Hz, 1H).

The synthetic route of 3,6-Dichloro-1,2,4,5-tetrazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BENDER, John A.; GENTLES, Robert G.; PENDRI, Annapurna; WANG, Alan Xiangdong; MEANWELL, Nicholas A.; BENO, Brett R.; FRIDELL, Robert A.; BELEMA, Makonen; NGUYEN, Van N.; YANG, Zhong; WANG, Gan; KUMARAVEL, Selvakumar; THANGATHIRUPATHY, Srinivasan; BORA, Rajesh Onkardas; HOLEHATTI, Shilpa Maheshwarappa; METTU, Mallikarjuna Rao; PANDA, Manoranjan; (319 pag.)WO2016/172424; (2016); A1;,
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. 1435-44-5, name is 1-Chloro-2,4-difluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Chloro-2,4-difluorobenzene

(a) 3-Chloro-2,6-difluorobenzaldehyde n-Butyllithium (1.43M in hexane, 20.2 mmol, 14.1 ml) was added dropwise at 0 C. to a solution of diisopropylamine (2.91 ml, 22.2 mmol) in THF (80 ml). After 30 min. at 0 C., the solution was cooled to -78 C. and 1-chloro-2,4-difluorobenzene (3 g, 20.2 mmol) in THF (10 ml) added dropwise. After 30 min., 4-formylmorpholine (4.1 ml) was added and the mixture warmed to room temperature over 1 h, diluted with 1N HCl, extracted twice with ethyl acetate, the extracts washed with brine, dried over sodium sulphate and evaporated to give a mobile yellow oil (2.2 g), MS (+EI) 178/177/176/175 (M+), 1H NMR (CDCl3) 10.34 (1H, s), 7.66-7.60 (1H, m), 7.00 (1H, dt, J6.9 Hz, 1.2 Hz).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1435-44-5.

Reference:
Patent; Astra Pharmaceuticals Limited; US5883102; (1999); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 13918-92-8, 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: The target compound 10a was obtained by treating 9a (533 mg, 1 mmol) with BF3xEtO2 (2 mL, 1.5 mmol) in CH2Cl2 in first step, the crude deprotected compound was directly reacted with methyl sulfonyl chloride (1.2 ml, 1 mmol) in the presence of triethyl amine (3.3 mL, 3 mmol) in dry THF (50 ml). After stirring the reaction mixture for 6 h, the reaction mixture was poured on to crushed ice (1.4 g) and the reaction mixture extracted and purified by column chromatography affords final product 10a as yellow solid.

The synthetic route of 2,4-Difluorobenzene-1-sulfonyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bharath, Yarlagadda; Alugubelli, Gopi Reddy; Sreenivasulu, Reddymasu; Rao, Mandava. V. Basaveswara; Chemical Papers; vol. 72; 2; (2018); p. 457 – 468;,
Chloride – Wikipedia,
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Electric Literature of 64628-73-5, The chemical industry reduces the impact on the environment during synthesis 64628-73-5, name is 3-Chloro-4-(trifluoromethoxy)aniline, I believe this compound will play a more active role in future production and life.

EXAMPLE 8 Production of N-(3-chloro-4-trifluoromethoxyphenyl)-1-methylcyclopropanecarboxamide (Compound No. 6): To a solution of 3-chloro-4-trifluoromethoxyaniline (2.1 g) in methylene chloride (50 ml), triethylamine (1.1 g) was added, and a solution of 1-methylcyclopropanecarbonyl chloride (1.2 g) in methylene chloride was dropwise added thereto while stirring and ice-cooling. After stirring at room temperature for 1 hour, the reaction mixture was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated. The crude crystals (2.9 g) were recrystallized from ethanol to give N-(3-chloro-4-trifluoromethoxyphenyl)-1-methylcyclopropanecarboxamide (2.6 g). M.P., 101-102 C. Anal. Calcd. for C12 H11 ClF3 NO2: C, 49.08%; H, 3.78%; N, 4.77%; Cl, 12.07%. Found: C, 48.92%; H, 3.81%; N, 4.60%; Cl, 12.30%. NMR deltaCDCl 3 (ppm): 0.75 (2H, m), 1.30 (2H, m), 1.46 (3H, s), 7.3 (2H, m), 7.54 (1H, br. s), 7.76 (1H, d, J=2 Hz).

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, 3-Chloro-4-(trifluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sumitomo Chemical Company, Limited; US4447260; (1984); A;,
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. 10061-02-6, name is trans-1,3-Dichloropropene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C3H4Cl2

To a 500 ml round bottom flask was charged 7-fluoro-6-nitrobenzoxazin-3-one (12.73 g, 0.060 mol) and potassium carbonate (9.95 g, 0.072 mol)Dissolved in 60 ml of N,N-dimethylformamide to form a suspension,Heating to 80 C,After the reaction was kept at this temperature for 30 minutes,(E)-1,3-dichloropropene (8.00 g, 0.072 mol) was added dropwise thereto.The reaction was maintained at 80 C for an additional 4 hours. After stopping the reaction,Cool naturally to room temperature and pour into 200 ml of water.After extraction with ethyl acetate (100 ml × 3), the combined organic phases were washed with saturated aqueous sodium chloride (50 ml × 3), dried over anhydrous magnesium sulfate Ester: petroleum ether = 1:3) 12.20 g of (E)-4-(3-chloroallyl)-7-fluoro-6-nitrobenzoxazin-3-one as a yellow solid, yield 71 %.

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shenyang Sinochem Pesticide Chemical Research And Development Co., Ltd.; Li Bin; Chen Lin; Cui Dongliang; Guo Zhengfeng; Ma Hongjuan; Lian Weixiang; (23 pag.)CN109836393; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 698-01-1, name is 2-Chloro-N,N-dimethylaniline, 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. Application In Synthesis of 2-Chloro-N,N-dimethylaniline

General procedure: In to an oven-dried flask, N,N-dimethylaniline 1a(2.0 mmol), 1-(isocyanomethylsulfonyl)-4-methylbenzene 2a (1.0mmol), CuCl (0.2 mmol), PPh3 (0.4 mmol), SDS (0.5 mmol) and TBHP (70wt% aqueous, 2.7 mmol) were added at room temperature. In open air, water (5mL) was added and the reaction mixture was allowed to reaction at 70 oCfor 6 h. After the finish of the reaction, the mixture was filtered through apad of celite and the filtrate was extracted by EA three times. The combined organic layers was washed by brine and dried by Na2SO4. Afterthe removing of the organic solvents, the residue was then separated on a silica gel column and the final product was obtained as a yellow powder (174 mg, 52%).

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

Reference:
Article; Xie, Chunsong; Han, Laihong; Tetrahedron Letters; vol. 55; 1; (2014); p. 240 – 243;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics