Category: chlorides-buliding-blocks

Reference of 870-24-6, The chemical industry reduces the impact on the environment during synthesis 870-24-6, name is 2-Chloroethanamine hydrochloride, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of the corresponding pyrrole or indole derivative (10 mmol) in MeCN (30 ml) was added sodium hydroxide (2.00 g, 50 mmol) and tetrabutylamonium hydrogen sulfate (0.17 g, 0.5 mmol). After the solution was stirred at room temperature for 30 min, 2-chloroethylamine hydrochloride (1.39 g, 12 mmol) was added. Then the reaction mixture was refluxed for 24 h. The mixture was poured into water (100 ml), extracted with diethyl ether, dried under MgSO4, and concentrated under reduced pressure to give a crude product. The crude was then purified by flash column chromatography on silica gel (eluted with petroleum ether / ethyl acetate=1 : 1) to give the pure product.

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

Reference:
Article; Tian, Yu-Ting; Zong, Yu-Wei; Nie, Jing; Zhang, Fa-Guang; Ma, Jun-An; Journal of Fluorine Chemistry; vol. 226; (2019);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1939-99-7,Some common heterocyclic compound, 1939-99-7, name is Phenylmethanesulfonyl chloride, molecular formula is C7H7ClO2S, 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.

A solution of phenylmethanesulfonyl chloride (2.19 g, 10 mmol) was added into asuspension of 3-bromopropan-1-amine hydrobromide (2.19 g, 10 mmol) and Et3N (2.02 g, 20 mmol) in THF (50 mL) at 0 C. The mixture was stirred at 0 C for 5 mm. TLC confirmed the completion of reaction. Solid was filtered out with suction, and the filtrate was concentrated toprovide compound N-(3-bromopropyl)(phenyl)methanesulfonamide (2.7 g, quant.) as a paleyellow solid which was used in the next step without further purification. ?H NMR (300 MHz, CDC13) oe 7.40 (m, 5H), 4.48 (m, 1H), 4.27 (s, 2H), 3.41 (t, J = 6.6 Hz, 2H), 3.16 (q, 2H), 2.01 (m, 2H). LCMS (ESI), mlz, 314 and 316 [M+Naj, Br pattern found.

The synthetic route of 1939-99-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; RENE, Olivier; FAUBER, Benjamin; VESEY, David; WINSHIP, Paul; LADDUWAHETTY, Tammy; (97 pag.)WO2017/5668; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 384-16-7, name is 2-Bromo-1-chloro-3-(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 384-16-7, Formula: C7H3BrClF3

Under nitrogen substitution,2-Bromo-3-chlorobenzotrifluoride (212 mg)Of tetrahydrofuran (0.7 mL)Was added isopropyl magnesium chloride / lithium chloride complex / tetrahydrofuran solution (1.3 M, 0.63 mL) dropwise at room temperature and stirred for 1 hour.This solution was added to the ice-cooled compound (172 mg) obtained in Example 46c,In diethyl ether (3 mL) over 5 minutes.Thereafter, the mixture was stirred under ice-cooling for 2 hours and at room temperature for 2.5 hours.Since the reaction was not completed,Again 2-bromo-3-chlorobenzotrifluoride (212 mg),From isopropyl magnesium chloride / lithium chloride complex / tetrahydrofuran solution (1.3 M, 0.63 mL)Grignard reagent was prepared by the same operation as above,Was added dropwise to the ice-cooled reaction solution over 5 minutes.After stirring for 1 hour under ice cooling, 0.5N hydrochloric acid was added and the mixture was extracted with ethyl acetate.The extract layer was washed successively with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine,After drying with anhydrous sodium sulfate and filtration, the solvent was distilled off under reduced pressure.The obtained residue was purified by silica gel column chromatography (ethyl acetate / hexane) to obtain the title compound (71.0 mg) as a colorless transparent gummy solid.

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Reference:
Patent; DAIICHI SANKYO COMPANY LIMITED; NAGAMOCHI, MASATOSHI; KOZAWA, YUJI; INAGAKI, HIROAKI; GOTANDA, KENTOKU; NOGUCHI, TETSUJI; TORIHATA, MUNEFUMI; YOSHINO, TOSHIHARU; ISOBE, TAKASHI; (113 pag.)JP2016/141632; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 16793-91-2, These common heterocyclic compound, 16793-91-2, name is 2-Chlorophenethyl Bromide, 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: General synthetic procedure for the final products.The appropriately substituted 4-phenethylpiperidine (6)(0.5 mmol) was dissolved in acetonitrile (5 mL) and K2CO3(0.75 mmol) and the appropriate phenethyl bromide (7) (0.5 mmol) added. The reaction mixture was refluxedfor 8 h.After completion of the reaction (monitored by TLC), the reaction mixture was cooled to ambient temperature and filtered through a Celite pad. The filtrate was concentrated under vacuum to obtain the desired crude product. The crude product was further purified by column chromatography (silica gel: 3-5% methanol in dichloromethane) to afford the corresponding 1,4-diphenethylpiperidine (8a-8y) in good yield (75-80 %), which was then converted to hydrochloride salt by treatment with 2M HCl in diethyl ether.Compounds12a-12dwere synthesized using the same procedure as above, except that an appropriately substituted 4-benzylpiperidine (11) was utilized in place of compound6.

Statistics shows that 2-Chlorophenethyl Bromide is playing an increasingly important role. we look forward to future research findings about 16793-91-2.

Reference:
Article; Nickell, Justin R.; Culver, John P.; Janganati, Venumadhav; Zheng, Guangrong; Dwoskin, Linda P.; Crooks, Peter A.; Bioorganic and Medicinal Chemistry Letters; vol. 26; 13; (2016); p. 2997 – 3000;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 10061-02-6, These common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, 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.

Potassium hydroxide (32.2 g) and toluene (250 mL) were taken into a round bottom flask and stirred for about 10 minutes. Dimethylisopropyl malonate (50 g) and tetrabutylammonium bromide (10 g) were then added to it and again stirred for about 10 minutes, trans-lambda ,3-Dichloropropene (35 g) was added to the reaction mixture and maintained at about 30-35 C for about 4 hours. After the reaction was completed, the reaction mass was quenched with water (500 ml_) and stirred for about 10 minutes. The reaction mixture was extracted into toluene (250 ml_), and the toluene layer was washed with water and then evaporated under reduced pressure to afford 51 g (82% yield) of (£)-dimethyl 2- (3-chloroallyl)-2-isopropylmalonate as a dark brown viscous liquid. Purity by GC: 96.84%

Statistics shows that trans-1,3-Dichloropropene is playing an increasingly important role. we look forward to future research findings about 10061-02-6.

Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; KOLLA, Naveen Kumar; APPAYE, Kaliyaperumal Srinivasan; GANGULA, Srinivas; GOVINDAPUR, Rajeshwar Reddy; MANNE, Nagaraju; NIKUMBH, Satish Pandurang; NEELAM, Uday Kumar; JOSEPH, Suju Chuttippari; BADDAM, Sudhakar Reddy; KUNHIMON, Shyam Kumar Unniaranpurakkal; MOOVENDAN, Mohan; DAHANUKAR, Vilas; DONIPARTHI, Kiran Kumar; WO2012/21446; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 6276-54-6, 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. 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: 2-Chlorobenzylamine (14.2 g, 0.10 mol), 4-chlorobenzylamine (14.2 g, 0.10 mol), and2,4-dichlorobenzylamine (17.6 g, 0.10 mol) were each dissolved in water (100 cm3),together with phosphorous acid (16.5 g, 0.20 mol), and concentrated hydrochloric acid (d1.18) (100 cm3) was added. The mixture was heated under reflux on a water bath (100C)and formalin (37% aqueous formaldehyde) (0.20 mol) was added portionwise. After 1 hwater was removed by evaporation until crystals appeared. The solution was then cooledand the product was filtered off and recrystallized three times from water to give theproduct as a white crystalline solid, as follows.

The chemical industry reduces the impact on the environment during synthesis 3-Chloropropan-1-amine hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Article; Hudson, Harry R.; Koroma, Sia N.; Ojo, Isaac A. O.; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 190; 12; (2015); p. 2187 – 2193;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2687-12-9, 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. 2687-12-9, name is Cinnamyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a well-stirred solution of 6a-e (1 mmol) in 4 mL of dry DMF was added the suitable organic halides (5.0-6.0 mmol) followed by K2CO3 (5.0-8.0 mmol) and the reaction mixture was heated at 70-80 C with stirring until the reaction was completed. The progress of the reaction was checked by TLC, which showed the appearance of new spots with higher Rf value than the starting compound. After the completion of the reaction, water was added to it and extracted with dichloromethane, washed successively with water and brine and then dried over anhydrous Na2SO4. The residue after solvent evaporation in vacuo, was purified by silica gel column chromatography (10% EtOAc : hexane). cis-3-pentyl-1,4-diphenyl-3-phenylsulfonyl-beta-lactam 7d

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, Cinnamyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Bhalla, Aman; Modi, Garima; Yadav, Pooja; Kumar, Pankaj; Bari; Hundal, Geeta; Tetrahedron Letters; vol. 61; 29; (2020);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 627-42-9, These common heterocyclic compound, 627-42-9, name is 2-Methoxyethyl chloride, 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 excess of n-BuLi (2.5 M in n-hexane; 1.0 mL, correct stoichiometric amount corresponding to 0.50 mL, 1.24 mmol) was added via cannula through a rubber septum to a flask containing N,N-bis(2-phosphinoethyl)methoxyethylamine (5′) (60 mg, 0.31 mmol) in freshly distilled THF (10 mL) at 0 C. The solution became dark (black-violet coloured). Still at 0 C., under stirring, 2-chloroethyl methylether (236 mg, 2.48 mmol) dissolved in distilled THF (5 mL) was added dropwise. The mixture was left to reach room temperature overnight becoming yellow-gold coloured. It was then reduced to one third of the initial volume by a gentle stream of dinitrogen. Distilled diethylether (20 mL) was added. The flask was cooled again with an ice bath and degassed water (5 mL) was added dropwise. Two phases were formed: the upper organic phase was yellow-gold coloured, whereas the aqueous phase was almost colourless. Degassed diethylether (20 mL) was added, and the mixture was transferred in a separatory funnel (previously fluxed with dinitrogen) via cannula to avoid the contact with the atmosphere. Always under a dinitrogen atmosphere the lower aqueous phase was recovered in another separatory funnel and treated with additional diethylether (2×10 mL). Then the aqueous phase was discharged and the combined ethereal phases were placed in a 100 mL round bottom flask containing anhydrous Na2SO4 (ca. 500 mg). The solid was filtered off under dinitrogen and washed with additional anhydrous diethylether (2×10 ml). The combined ethereal phases were concentrated under dinitrogen and then under vacuum (yield ca. 60%).1H NMR (CDCl3): delta(ppm)=3.57-3.47 (10H); 3.33 (s, 12H); 3.32 (s, 3H); 2.66 (m, 6H); 1.78 (t, 8H); 1.65 (m, 4H).13C NMR (CDCl3): delta(ppm)=71.02 (s); 70.39 (d); 58.86 (s); 52.48 (s); 52.52 (s); 50.83 (d); 27.96 (d); 24.75 (d).31P{1H} (CDCl3): delta(ppm)=-39.0.

The synthetic route of 627-42-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NIHON MED-PHYSICS CO., LTD.; US2010/160615; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 933190-51-3, These common heterocyclic compound, 933190-51-3, name is 8-Bromo-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.

General procedure: To a solution of 6a-6c (1 mmol) in THF (5 mL) was addedmorpholine (or (S)-3-methylmorpholine, or 8-oxa-3-azabicyclo[3.2.1]octane) (1.2 mmol) and Et3N (2.2 mmol). The mixture washeated under reflux for 12 h. The crude product was extracted with CH2Cl2, dried over Na2SO4, purified over silica gel chromatographyeluting with PE and EtOAc to give 7a-7g [43].

Statistics shows that 8-Bromo-6-chloroimidazo[1,2-b]pyridazine is playing an increasingly important role. we look forward to future research findings about 933190-51-3.

Reference:
Article; Mao, Beibei; Gao, Shanyun; Weng, Yiran; Zhang, Liangren; Zhang, Lihe; European Journal of Medicinal Chemistry; vol. 129; (2017); p. 135 – 150;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 74483-46-8,Some common heterocyclic compound, 74483-46-8, name is 2-Chloro-4-methyl-1-(trifluoromethyl)benzene, molecular formula is C8H6ClF3, 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.

Intermediate 4: 4-(Bromomethyl)-2-chloro-1-(trifluoromethyl)benzene; To a solution of 2-chloro-4-methyl-1-(trifluoromethyl)benzene (0.5g, 2.57 mmol) in dry carbone tetrachloride (5OmL), N-bromo succinimide (0.412g, 2.313mmol) and benzoyl peroxide (12mg, 0.05 mmol) were added. The reaction was stirred to reflux for 40 hours. After cooling at 00C, the reaction mixture was filtered and the solvent evaporated. The title compound was obtained (0.7g) and the crude compound was used in the next reaction without purification. GC/MS: m/z, 273 Rt: 5.5 min

The synthetic route of 74483-46-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2009/16216; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics