Category: chlorides-buliding-blocks

Reference of 2106-02-7,Some common heterocyclic compound, 2106-02-7, name is 2-Chloro-4-fluoroaniline, molecular formula is C6H5ClFN, 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 150-mL round-bottomed flask containing Compound 9 (0.5 g, 2.2 mmol) in 15 mL of CH2CI2, was added 2-chloro-4-fluoroaniline (0.33 g, 2.3 mmol) and pyridine (2 mL). The reaction mixture was stirred at room temperature for 2 hours. Evaporation of the solvents in vacuo gave an oily material, which was dissolved in EtOAc (15 mL), and the organic phase was separated and washed with 5% brine, dried over Na2SO4. Filtration and evaporation in vacuo gave title Compound 10 (0.7 g, 94%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-4-fluoroaniline, its application will become more common.

Reference:
Patent; TAIWANJ PHARMACEUTICALS CO., LTD; YANG, Syaulan S.; LEE, Kuang-Yuan; LIU, Meng-Hsien; HSIAO, Ming-Yu; PENG, Huang-Kai; WANG, Chiung-Wen; WU, Edwin SC; CHIU, Peter JS; (77 pag.)WO2018/156297; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 6775-78-6, These common heterocyclic compound, 6775-78-6, name is 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.

Intermediate A 3-Bromo-6-chloroimidazo[1 ,2-b]pyridazine intermediate A To a solution of 6-chloroimidazo[1 ,2-b]pyridazine (5 g, 32.6 mmol) in acetonitrile (300 ml) was added 1-bromopyrrolidine-2,5-dione (6.37 g, 35.8 mmol) and trifluoroacetic acid (0.75 mL). The resulting solution was allowed to stirr at room temperature overnight. The solvent was removed under reduced pressure and the residue was dissolved in EtOAc, washed with NaHCOs solution, water and brine, dried over Na2SO4 and concentrated in vacuo to afford 7.2 g title compound in 92% yield as a light yellow solid. 1H-NMR (400MHz, CDCI3) delta ppm 7.91 (d, 1 H), 7.79 (s, 1 H), 7.12 (d, 1 H). LCMS (method A): [MH]+ = 232/234, tR = 4.48 min.

Statistics shows that 6-Chloroimidazo[1,2-b]pyridazine is playing an increasingly important role. we look forward to future research findings about 6775-78-6.

Reference:
Patent; NOVARTIS AG; FU, Xingnian; HE, Feng; LI, Yue; LIU, Lei; MI, Yuan; XU, Yao-chang; XUN, Guoliang; YU, Zhengtian; ZHANG, Ji Yue (Jeff); DAI, Miao; WO2011/18454; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 4090-55-5, These common heterocyclic compound, 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, 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.

(Synthesis of phosphorus compound (5)); The flask accommodating the post-reaction solution containing intermediate 6 was filled with 80.8 g (0.8 mol) of triethylamine, 4.1 g (0.034 mol) of 4-(dimethylamino) pyridine, and 420 g of 1, 2-dichloroethane. While the mixed solution was stirred, a mixed solution of 123.6 g (0 .67 mol) of material 1 and 450 g of 1,2-dichloroethane was added thereto at 20C over 2 hours. After that, the substances were reacted at the same temperature (20C) for 8 hours. The obtained post-reaction solution was neutralized at room temperature using an aqueous solution of hydrochloric acid in an amount corresponding to the excess amount of triethylamine and the amount of sodium methoxide used for synthesizing intermediate 6. The resultant solution was kept still so as to be separated into different layers. Then, the organic layer was neutralized using an aqueous solution of sodium hydrogen carbonate. The organic layer was then washed with water twice. The obtained organic layer was dried by anhydrous magnesium sulfate. The solvent and water were removed by distillation, thereby obtaining 212.9 g of phosphorus compound (5). Phosphorus compound (5) had a purity measured by GPC (gel permeation chromatography) of 82.0% by area. The yield was 62.1%.

Statistics shows that 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide is playing an increasingly important role. we look forward to future research findings about 4090-55-5.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1632497; (2006); 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. 621-62-5, name is 2-Chloro-1,1-diethoxyethane, A new synthetic method of this compound is introduced below., Computed Properties of C6H13ClO2

COMPARATIVE EXAMPLE 1 Preparation of 2-benzoyloxyacetaldehyde diethyl acetal Chloroacetaldehyde diethyl acetal (1.9 g), potassium benzoate (2.0 g) and DMF (20 mL) were placed in a three-neck flask, followed by refluxing. Twenty hours later, the reaction mixture was cooled to room temperature, and water (60 mL) and ethyl acetate (80 mL) were added thereto, followed by stirring. After filtration and separation, the organic layer was concentrated and thereby yielded the target compound (0.69 g) in a yield of 30%. While the present invention has been described with reference to what are presently considered to be the preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments. On the contrary, the invention is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. The scope of the following claims is to be accorded the broadest interpretation so as to encompass all such modifications and equivalent structures and functions.

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; Daicel Chemical Industries, Ltd.; US2005/234246; (2005); 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. 14490-19-8, name is 1,4-Dichloropyrido[3,4-d]pyridazine, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H3Cl2N3

To a round bottomed flask were added tert-butyl piperidin-4-ylmethylcarbamate (0.29mL, 55mmol)1 ,4-dichloropyrido[3,4-d]pyridazine (1 3.48mL, 5Ommol) , N,N-diisopropylethylamine (26mL,1 5Ommol) , NMP (50mL) and heated to 100C for 1 hour. The reaction was diluted with EtOAc andwashed with water (5×1 OOmL). The organic layer was dried over sodium sulphate, filtered andconcentrated in vacuo. The resulting residue was purified by silica flash chromatography using 30%EtOAc in heptane using a slow isocratic elution and concentrated in vacuo to afford the majorregioisomer tert-butyl N-[1 -(1 -chloropyrido[3,4-d]pyridazin-4-yl)-4-piperidyl]-N-methyl-carbamate(1 .lg, 2.9mmol, 5.8%, 98% purity). Further mixed fractions of lower purity were also obtained.1H NMR (400MHz, ODd3) s/ppm: 9.46 (s, 1 H), 9.03 (d, J5.6Hz, 1 H), 7.94 (d, J5.6Hz, 1 H), 4.33(m(br), 1H), 4.22-4.12 (m(br), 2H), 3.29 (t, J12.5Hz, 2H), 2.83 (s, 3H), 2.11-1.97 (m, 2H), 1.90-1.81(m, 2H), 1.50 (s, 9H).MS Method 2: RT: 1 .73mm. m/z 378.9[M÷H]

According to the analysis of related databases, 14490-19-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; REDX PHARMA LIMITED; ARMER, Richard; BINGHAM, Matilda; BHAMRA, Inder; MCCARROLL, Andrew; WO2014/191737; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 57946-56-2, A common heterocyclic compound, 57946-56-2, name is 4-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.

[0146] Sodium nitrite (2.35 g, 34.13mmol) solution (40 mL) was added dropwise to 4- Chloro-2-fluoro aniline (4. [5G,] 31mmol) in 170 mL HBr [AT-10C] bath temperature, then the mixture was stirred for 30 min at-10C bath temperature. In parallel, copper sulfate (10.22g, 24. [29MMOL)] and sodium bromide (3.79 g, 36. [8MMOL)] were mixed and the reaction mixture was heated at [60C] for 30 min. Then sodium sulfite (2.66g, 21. [2MMOL)] was added into this copper sulfate reaction mixture and heated for [95C] for 30 min. The reaction mixture was cooled to room temperature and solid formed was washed with water to afford white solid cuprous bromide. The diazonium salt was portion wise added into the freshly prepared cuprous bromide in 40 mL HBr [AT-10C] bath temperature and the reaction mixture was then warmed to room temperature. The reaction mixture was heated at [55C] for 20 min, cooled and then extracted with ethyl acetate three times. The combined organic layer was washed with water and saturated brine solution, dried over sodium sulfate and concentrated. The crude material was purified by column chromatography (5: 95 ethyl acetate: pet ether) to afford solid product.

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; CHEMOCENTRYX, INC.; WO2003/105853; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 622-24-2, name is (2-Chloroethyl)benzene, 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. Recommanded Product: 622-24-2

To the reaction flask by adding material five, substance six, dimethyl formamide, potassium carbonate, reaction, Cooled to 25 C, The reaction solution was added to ice water, The mass of the ice water was 10 times of that of the reaction solution, filter, Washed, Drying, Substance seven was obtained

The synthetic route of (2-Chloroethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; China Three Gorges University; Tan, Xiao; Liu, Sen; Yang, Liting; (21 pag.)CN106214681; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 694-80-4, name is 1-Bromo-2-chlorobenzene, molecular formula is C6H4BrCl, 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: 694-80-4

General procedure: In a Schlenk flask under N2 atmosphere, 2a (5 mg, 0.011 mmol), PdCl2 (2 mg, 0.011 mmol), Cs2CO3 (358 mg, 1,1 mmol) and DMF(1.5 mL) were added. The reaction mixture was heated at 90 C for 30 min. Then, an aryl halide (1.0 mmol) and an olefin (1.2 mmol)were added and the mixture was further stirred at 125 C under air atmosphere conditions. The reaction progress was monitored by Thin Layer Chromatography (EtOAc/hexane, 1:9). After completion of the reaction, the mixture was cooled to room temperature, and water (8 mL) was added and was extracted with EtOAc (3 10 mL).The organic solvent was dried over Na2SO4 and was evaporated under vacuum to give the crude product which was further purified by column chromatography using EtOAc/hexane, 1:9.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 694-80-4, its application will become more common.

Reference:
Article; Takallou, Ahmad; Habibi, Azizollah; Halimehjani, Azim Ziyaei; Balalaie, Saeed; Journal of Organometallic Chemistry; vol. 888; (2019); p. 24 – 28;,
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. 870-24-6, name is 2-Chloroethanamine hydrochloride, A new synthetic method of this compound is introduced below., Product Details of 870-24-6

4-Methoxythiophenol (50 g, 0.357 mol), 2-chloroethylamine monohydrochloride (39.8 g, 0.343 mol.), K2CO3(78.8 g, 0.57 mol) and diisopropyl ethylamine (32 mL, 0.178 mol) were mixed in 200 mL of THF. The mixture was degassed for 5 min. under reduced pressure and refluxed under argon overnight. The solvent was removed and water (300 mL) was added to the flask. The mixture was extracted with dichloromethane (3*200 mL). The organics were collected, dichloromethane was removed and 50 mL conc. HCl was added, followed by 200 mL of water. The solution was extracted with 1:1 EtOAc/hexane (3*200 mL). The aqueous layer was adjusted to pH 10 with 2 M NaOH, and was extracted with dichloromethane (3*200 mL). The combined organic solution was dried over anhydrous sodium sulfate. Removal of solvent provided 61 g of the target compound as a colorless liquid, with a yield of 97%. 1H-NMR (300 MHz, CDCl3): 7.35 (d, J=8.7 Hz, 2H), 6.81 (d, J=8.7 Hz, 2H), 3.77 (s, 3H), 2.88-2.80 (m, 4H), 1.44 (s, 2H).

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; Deng, Shixian; Belvedere, Sandro; Yan, Jiaming; Landry, Donald; US2009/227788; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, HPLC of Formula: C3H4Cl3NO

A mixture of 1.98 g of 4-trifluoromethylbenzene-1, 2-diamine and 15 ml of acetic acid was added to a mixture of1.98 g of methyl-2,2,2-trichloroacetimidate and 15 ml of acetic acid under ice cooling, followed by stirring for 3 hours at room temperature. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residues, and the resultant was washed with an aqueous saturated sodium hydrogen carbonate solution and saturated saline. The organic layer was dried over magnesium sulfate and then concentrated under reduced pressure, thereby obtaining 3.39 g of 2-trichioromethyl-5-trifluoromethylbenzimidazole. 1H-NMR (DMSO-D5) oe: 8.18-8.00 (m, 1H), 7.94-7.80 (m, 1H), 7.72-7.65 (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, Methyl 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; Mukumoto, Fujio; Tamaki, Hiroaki; Kusaka, Shintaro; Iwakoshi, Mitsuhiko; US2015/289512; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics