Chlorides-buliding-blocks

Synthetic Route of 108-37-2, 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. 108-37-2, name is 1-Bromo-3-chlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of diisopropylamine (76 mL, 0.4 mol) in anhydrous THF (664 mL) and n-hexane (220 mL) was added 2.5 M n-BuLi (160 mL, 0.4 mol) dropwise at -78 0C over 1 h. The mixture was stirred for 1 h at -78 0C and a solution of 1-bromo- 3-chlorobenzene (76 g, 0.4 mol) in anhydrous THF (300 mL) was added dropwise at – 78 0C. After stirring for an additional 1 h at the same temperature, a solution of iodine (101 g, 0.4 mol) in anhydrous THF (400 mL) was added dropwise at -78 0C. The temperature was raised from -78 0C to rt during 2 h. After stirring for 18 h at rt, the mixture was concentrated in vacuo to give the crude product (120 g) which was distilled under reduced pressure to give l-bromo-3-fluoro-2-iodobenzene (115 g, 91%). 1H NMR (400MHz, CDCl3): 7.12-7.18 (t, IH), 7.35-7.41 (dd, IH), 7.49-7.54 (dd, IH); MS (E/Z): 317 (M+H+)

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

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; VITAE PHARMACEUTICALS, INC.; WO2008/124575; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 53531-69-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 53531-69-4 name is (4-Bromophenyl)methanesulfonyl chloride, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a stirred solution of (4-bromophenyl)methanesulfonyl chloride (DC; 500 mg, 1.85 mmol) in pyridine (10 mL) under inert atmosphere was added morpholine (712 mg, 2.22 mmol) at RT and stirred for 16 h. The reaction was monitored by TLC. After complete consumption of the starting material, the reaction mixture was diluted with water (30 mL) and was extracted with EtOAc (2×20 mL). The combined organic extracts were washed with water (15 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure to obtain the crude. The crude was purified by silica gel column chromatography (20-30% EtOAc/hexanes) to afford DD (360 mg, 61%) as a white solid. *H NMR (400 MHz, CDC13): delta 7.53 (d, J = 8.8 Hz, 2H), 7.29 (d, / = 8.8 Hz, 2H), 4.16 (s, 2H), 3.65 (t, / = 4.8 Hz, 4H), 3.13 (t, 7 = 4.8 Hz, 4H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (4-Bromophenyl)methanesulfonyl chloride, and friends who are interested can also refer to it.

Reference:
Patent; VIAMET PHARMACEUTICALS, INC.; HOEKSTRA, William, J.; YATES, Christopher, M.; RAFFERTY, Stephen, W.; WO2014/117090; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 1939-99-7 as follows. Recommanded Product: 1939-99-7

Example 95 Preparation of t-Butyl (3-Benzylsufonylamino-6-methyl-2-oxo-1,2-dihydro-1-pyridyl)acetate STR115 Collidine (0.59 mL, 4.5 mmole) was added in one portion to a stirred solution of the compound of Example 94 (0.89 g, 3.7 mmole) and benzylsulfonyl chloride (0.86 g, 4.5 mmole) in acetonitrile (20 ml) cooled in an ice bath. The solution was stirred for 5 minutes at 0 C., followed by 45 min at room temperature. The reaction mixture was quenched with water, then diluted with ethyl acetate (100 mL), washed with 3% HCl (until aqueous layer is pH 1), and brine, dried over magnesium sulfate, and the solvent was removed. The residue was dissolved in methanol, concentrated to a volume of approximately 3 mL, and the product was precipitated with the addition of diethyl ether. The precipitate was filtered to give 0.67 g of the title compound. The filtrate was concentrated and chromatographed on flash silica gel using 20-67% ethyl acetate hexanes as eluent. An additional 0.20 g of the title compound was recovered. A total of 0.87 g of the title compound (59% yield) was recovered. Rf=0.29 (silica gel, 33% ethyl acetate/hexanes).

According to the analysis of related databases, 1939-99-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Corvas International, Inc.; US5658930; (1997); A;,
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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Chloro-N,N-dimethylethanamine hydrochloride

l-(3′-Hydroxybenzenesulfonyl) indole (0.602 mmol, 0.163 grams) (obtained from preparation 1) was taken in 50 mL two neck round bottom flask and added tetrahydrofuran (7 mL). To the aboe mixture potassium carbonate (1.24 mmol, 0.171 grams) was added and stirred for a period of 15 – 20 minutes. The free base generated from 2-dimethylaminoethyl chloride hydrochloride (2.48 minol, 0.358 grams), by dissolving it in a solution of 3 mL 40 % aqueous sodium hydroxide, diluted with 5 mL water and extracting free base with toluene (3 mL) was directly charged to reaction mixture. Reaction mixture was kept on reflux temperature and the progress was monitored. After completion of reaction, the reaction mass was cooled to room temperature, poured onto 25 mL of water and extracted the product with ethyl acetate (10 mL x 4). Combined organic extracts were dried over sodium sulfate and the volatiles were removed under the reduced pressure to obtain 0.214 grams crude compound. The compound was purified by column chromatography using silica gel (100-200 mesh), the eluents being ethyl acetate and n-hexane (2:3) to obtain pure compound.IR (cm 1): 2947, 1373, 1 170;1H-NMR (ppm): 2.32 (6H, s), 2.70 – 2 .73 (2H, t, J = 5.57 Hz), 4.00 – 4.03 (2H, t, J = 5.58 Hz), 6.66 – 6.67 (IH, d, J = 3.33 Hz), 7.04 – 7.07 (IH, m); 7.20 – 7.24 (IH, m), 7.28 – 7.33 (2H, m),7.37 – 7.38 (I H, r), 7.43 – 7.48 (IH, m), 7.52 – 7.54 (IH, d, J = 7.94 Hz)5 7.54 – 7.55 (I H, d, J= 3.76 Hz), 7.97 – 7.99 (1 H, d, J = 8.29 Hz);Mass (m/z): 345 (M+H)

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; SUVEN LIFE SCIENCES LIMITED; WO2008/136017; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 698-01-1, 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. 698-01-1, name is 2-Chloro-N,N-dimethylaniline, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a stirred solution of tert-amines in dichloromethane (10 ml), m-chloroperbenzoic acid (70%w/w, 1.5 equiv) was added portion wise at room temperature. The resultant solution wasstirred for 4 h and the progress of reaction was monitored using TLC. After completion, the reaction mixture was directlyloaded on basic alumina column and purified using methanol:chloroform solvent mixture as an eluent. The combined filtrates were concentrated to give corresponding amine N-oxides with approx. 90-95% isolated yield.

The chemical industry reduces the impact on the environment during synthesis 2-Chloro-N,N-dimethylaniline. I believe this compound will play a more active role in future production and life.

Reference:
Article; Gupta, Surabhi; Sureshbabu, Popuri; Singh, Adesh Kumar; Sabiah, Shahulhameed; Kandasamy, Jeyakumar; Tetrahedron Letters; vol. 58; 10; (2017); p. 909 – 913;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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 20850-43-5, Product Details of 20850-43-5

REFERENCE EXAMPLE 2 Production of 2-[[(3,4-methylenedioxy)phenyl]methyl]malonic acid diethyl ester 60.17 g of sodium ethoxide were dissolved in 1127 ml of ethanol. To this solution, 336.4 g of diethyl malonate and 119.42 g of [(3,4-methylendioxy)phenyl]methyl chloride were added and the mixture was refluxed for 3 hours. After the reaction was completed, the solvent was removed under reduced pressure and water was added to the residue. After extraction with ethyl acetate, the ethyl acetate was dried with sodium sulfate anhydride. After removing the solvent under reduced pressure and purification with distillation, 181.1 g of 2-[[(3,4-methylenedioxy)phenyl]methyl]malonic acid diethyl ester were obtained.

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, 5-(Chloromethyl)benzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kaneka Corporation; US6121477; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 73006-78-7,Some common heterocyclic compound, 73006-78-7, name is 5-Chloro-[1,1′-biphenyl]-2-amine, molecular formula is C12H10ClN, 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 Method A: Synthesis of an isocyanate from an aniline To a solution of the aniline (5.21 mmol, 1.00 equivalent) in toluene (19.0 ml), triphosgene (0.35 equivalents) is added slowly and the reaction mixture is heated to reflux for 1 h. The reaction mixture is concentrated to dryness and the product is either purified by bulb-to-bulb distillation or used in the next step without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Chloro-[1,1′-biphenyl]-2-amine, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BUETTELMANN, Bernd; CECCARELLI, Simona M.; CONTE, Aurelia; KUEHNE, Holger; KUHN, Bernd; NEIDHART, Werner; OBST SANDER, Ulrike; RICHTER, Hans; WO2014/146994; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 309721-44-6, name is 2-Bromo-1-chloro-3-fluorobenzene, 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 309721-44-6, COA of Formula: C6H3BrClF

A mixture of 146.1 g (1.36 mol) of p-toluidine, 12.6 g (0.02 mol) of (+-)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl, 261.9 g (2.73 mol) of sodium t-butoxide, 314.1 g (1.50 mol) of 2-bromo-3-fluoro-chlorobenzene and 6.3 g (0.0069 mol) of tris(dibenzylideneacetone)dipalladium(0) in 3000 ml of toluene is heated to 110 over 30 minutes and stirred an additional 4 hours at this temperature. The mixture is cooled to room temperature and a solution of 680 ml 37% hydrochloric acid and 680 ml of water is added over 15 minutes. The mixture is stirred for 20 minutes and filtered through a pad of Celite. The layers are separated and the organic phase is washed twice with 680 ml of water and once with a solution of 225 g of sodium chloride in 680 ml of water. The solvents are evaporated under reduced pressure to give N-(2′-chloro-6′-fluorophenyl)-4-methylaniline as an oil, b.p. 129-131/0.5 mm Hg.

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-Bromo-1-chloro-3-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Novartis AG; US6291523; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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. Computed Properties of C8H11Cl2NO

Preparation of Compound IV:3-Chloro-4-methoxybenzylamine hydrochloride III (25.00 g, 0.12 mol)Suspended in 75mL acetonitrile,Add sodium bicarbonate (23.21 g, 0.27 mol),Compound II (22.02 g, 0.11 mol) was added,Stir at 40 degrees for 2.5 hours.The reaction solution was suction filtered,The filter cake was washed once with 10 mL of acetonitrile.Wash once with 10 mL of water.After the filter cake is dried by phosphorus pentoxide,32.01g of white solid compound IV,The yield was 87.37%.

The synthetic route of 3-Chloro-4-methoxybenzylamine Hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tierxi (Nanjing) Pharmaceutical Research And Development Co., Ltd.; Wu Wenchao; Song Dandan; Zhang Chi; Cui Xilin; (10 pag.)CN110117274; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4152-90-3, name is (3-Chlorophenyl)methanamine, 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 4152-90-3, Computed Properties of C7H8ClN

General procedure: To a solution of benzylamine (0.6 mmol), indole (1.0 mmol) and CuI (0.1 mmol ) in CH3CN (1 mL) was added TEMPO (0.15 mmol) under atmosphere and the mixture was stirred at room temperature for overnight. The reaction mixture was concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (eluent: EtOAc/PE = 1:4) to yield the corresponding product.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Liao, Meixiang; Zhang, Xiaoyun; Yue, Pengfei; Synthetic Communications; vol. 48; 13; (2018); p. 1694 – 1700;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics