Month: June 2021

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

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

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 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 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

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 2533-69-9, 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 2533-69-9 as follows.

2.00 g (12.0 mmol) Methyl-3,4-diamino-benzoate were dissolved in 50 ml concentrated acetic acid. Then 2.09 ml (1.4 equiv.) methyl-2,2,2-trichloroacetimidate were added slowly and the resulting mixture was stirred at room temperature for 2 h. The mixture was diluted with 100 ml toluene and the solvent was removed under reduced pressure. The residue was taken up in dichloromethane and washed once with a saturated NaHCO3-solution and once with brine. The organic layer was dried over MgSO4 and the solvent was removed under reduced pressure to give pure methyl-2-trichloromethyl-1H-benzoimidazole-5-carboxylate as a light brown amorphous solid. Yield: 3.64 g MS (ES+): m/e = 293, chloro pattern.

According to the analysis of related databases, 2533-69-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Aventis Pharma Deutschland GmbH; EP1479676; (2004); A1;,
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. 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, A new synthetic method of this compound is introduced below., Quality Control of 2,2,2-Trifluoro-N-phenylacetimidoyl chloride

1.46 g (1.45 mmol) VIII and 0.93 g (4.5 mmol)2,2,2-Trifluoro-N-phenyliminoacetyl chloride is dissolved in 30 mL of acetone,0.62 g (4.5 mmol) of potassium carbonate was added in portions and allowed to react at room temperature overnight.TLC (PE: EA = 2:1) was monitored and the reaction was completed.The reaction was quenched with 0.2 mL of methanol, filtered, and the filtrate was dried.Column chromatography (PE: EA = 4:1) gave 1.7 g of VI white solid, yield 99%.

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:
Patent; Shanghai Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Zhang Hongliang; Wang Zhefeng; Yi Bing; Wang Shengli; Liang Qian; Li Changsheng; (18 pag.)CN108299523; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 33050-38-3, A common heterocyclic compound, 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, molecular formula is C5H2Cl2N4, 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.

b) The 3-chloro-6-(morpholin-4-yl)[1,2,4]triazolo[4,3-b]pyridazine can be prepared in the following way:0.9 cm3 of morpholine and 1.4 cm3 of triethylamine are added to a solution of 1.89 g of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine in 20 cm3 of N,N-dimethylformamide. The reaction is stirred at 20 C. for 19 1H). 60 cm3 of water are added and the mixture is extracted with ethyl acetate. The organic phase is washed with water and with brine and then dried over magnesium sulphate and concentrated to dryness, to give a beige solid. The latter is chromatographed by solid deposit on a Merck cartridge of 70 g of silica 15-40 mum, elution being carried out with a gradient of 100% dichloromethane to 95/5 dichloromethane/methanol. 1.97 g of 3-chloro-6-(morpholin-4-yl)[1,2,4]triazolo[4,3-b]pyridazine are obtained in the form of a very pale yellow solid, the characteristics of which are as follows:MASS SPECTRUM: UPLC-MS-DAD-ELSD: 240=MH+.

The synthetic route of 33050-38-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; sanofi-aventis; US2010/298315; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics