Category: chlorides-buliding-blocks

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;,
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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;,
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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;,
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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

Related Products of 622-86-6, These common heterocyclic compound, 622-86-6, name is (2-Chloroethoxy)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.

2-(4-Nitrophenyl) butanoic acid (1.66 g, 7.9mmol) was dissolved in trifluoroacetic anhydride (1.1 mL, 7.9 mmol), then(2-chloroethoxy)benzene (1.0 ml, 7.2 mmol) was added dropwise. The resultingmixture was allowed to stir at room temperature overnight. The reaction mixture was poured into saturatedaqueous sodium bicarbonate solution (50 mL) and extracted with ethyl acetate (2x 50 mL). The combined organic phases were driedover anhydrous magnesium sulfate and concentrated on a rotaryevaporator. The resulting residue waspurified by chromatography on silica gel (ethyl acetate/hexane) to afford 1.49g (59%) of the desired compound as a white solid. 1HNMR (400 MHz, CDCl3) delta8.21 (d, J = 8.8 Hz, 2H), 7.96 (d, J = 8.9 Hz, 2H), 7.51 (d, J = 8.8 Hz, 2H),6.93 (d, J = 9.0 Hz, 2H), 4.56 (t, J = 7.3 Hz, 1H), 4.28 (t, J = 5.8 Hz 2H), 3.83 (t, J = 5.8 Hz, 2H),2.26 (m, 1H), 1.78 (m, 1H), 0.94 (t, J = 7.4 Hz, 3H); MS (ESI) (m/z) 348.1/350.1(M+H)+.

Statistics shows that (2-Chloroethoxy)benzene is playing an increasingly important role. we look forward to future research findings about 622-86-6.

Reference:
Article; Childers, Wayne; Fan, Rong; Martinez, Rogelio; Colussi, Dennis J.; Melenski, Edward; Liu, Yuxiao; Gordon, John; Abou-Gharbia, Magid; Jacobson, Marlene A.; Bioorganic and Medicinal Chemistry Letters; vol. 30; 2; (2020);,
Chloride – Wikipedia,
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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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene, A new synthetic method of this compound is introduced below., Product Details of 1996-30-1

2-Fluoro-5-chlorobromobenzene 18a (11.0 g, 52.8 mmol), ethynyltrimethylsilane (7.7 g, 79 mmol) and triethylamine (60 mL) were mixed together, and then cuprous iodide (100 mg, 0.53 mmol) and ditriphenylphosphine palladium chloride (1.86 g, 2.65 mmol) were added, the reaction mixture was heated to 80 C. under a nitrogen atmosphere and stirring was continued for 4 hours, after the reaction was completed, the solvent was removed from the solution under reduced pressure, the residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=100/1), so as to obtain the title product ((2-fluoro-5-chlorophenyl)ethynyl)trimethylsilane 18b (11.0 g, yellow oily substance), and the yield was 90%. 1H NMR (400 MHz, CDCl3) delta 7.45 (dd, J=6.0, 2.7 Hz, 1H), 7.28-7.22 (m, 1H), 7.02 (t, J=8.8 Hz, 1H), 0.29 (s, 9H).

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; BEIJING INNOCARE PHARMA TECH CO., LTD.; Chen, Xiangyang; Gao, Yingxiang; Kong, Norman Xianglong; (59 pag.)US2019/210997; (2019); A1;,
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Adding a certain compound to certain chemical reactions, such as: 60811-21-4, name is 4-Bromo-2-chloro-1-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 60811-21-4, Product Details of 60811-21-4

To an oven dried 8 mL vial with teflon cap purged with N2 was added Zinc dust (298 mg, 4.56 mmol), DMF(1.5 mL), and iodine (57.8 mg, 0.228 mmol). To this mixture was added (R)-methyl 2-((tert-butoxycarbonyl)amino)-3-iodopropanoate (500 mg, 1.519 mmol), immediately followed by iodine (57.8 mg, 0.228 mmol).Pd2(dba)3 (69.6 mg, 0.076 mmol), 2-dicyclohexylphosphino-2?6-dimethoxybiphenyl (62.4 mg, 0.152 mmol)and 4-bromo-2-chloro-1-fluorobenzene (477 mg, 2.279 mmol) were then added and the reaction mixture wasallowed to stir at 50 C. for 3 hours. The crude mixture was diluted in 30 mL of EtOAc and DMF wasremoved with 4 aqueous washes. The organic phase was dried over anhydrous sodium sulfate. The solutionwas filtered and concentrated, and the crude product was purified by silica gel chromatography using 100%hexanes to 30% EtOAc/Hexanes. The desired product was obtained as a pale yellow oil, (S)-methyl 2-((tert-butoxycarbonyl)amino)-3-(3-chloro-4-fluorophenyl)propanoate (0.174 g, 35%). 1H NMR (400 MHz,chloroform-d) delta 7.27 (s, 1H), 7.17 (dd, J=6.9, 1.4 Hz, 1H), 7.11-6.93 (m, 1H), 5.03 (d, J=6.8 Hz, 1H), 4.55(d, J=6.4 Hz, 1H), 3.73 (s, 3H), 3.19-3.04 (m, 1H), 2.98 (dd, J=13.9, 5.9 Hz, 1H), 1.49-1.37 (m, 10H).

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, 4-Bromo-2-chloro-1-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bristol-Myers Squibb Company; Miller, Michael Matthew; Mapelli, Claudio; Allen, Martin Patrick; Bowsher, Michael S.; Boy, Kenneth M.; Gillis, Eric P.; Langley, David R.; Mull, Eric; Poirier, Maude A.; Sanghvi, Nishith; Sun, Li-Qiang; Tenney, Daniel J.; Yeung, Kap-Sun; Zhu, Juliang; Reid, Patrick C.; Scola, Paul Michael; (892 pag.)US9308236; (2016); B2;,
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Electric Literature of 933190-51-3, The chemical industry reduces the impact on the environment during synthesis 933190-51-3, name is 8-Bromo-6-chloroimidazo[1,2-b]pyridazine, I believe this compound will play a more active role in future production and life.

Preparation of 6-chloro-N-cyclopropylimidazo[1,2-b]pyridazin-8-amine To a solution of 8-bromo-6-chloroimidazo[1,2-b]pyridazine (1.00 g, 3.21 mmol, 1.0 equiv) and p-TSA (611 mg, 3.21 mmol, 1.0 equiv) in DMSO (10.0 mL) was added cyclopropylamine (1.13 mL, 16.1 mmol, 5.0 equiv) and heated to 100 C. for 24 h. Purification by column chromatography using 50% ethyl acetate in hexanes elution gave 536 mg of the white solid, 80%.

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, 8-Bromo-6-chloroimidazo[1,2-b]pyridazine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Califia Bio, Inc.; GOODFELLOW, VAL S.; NGUYEN, THONG X.; RAVULA, SATHEESH B.; GELBARD, HARRIS A.; US2014/256733; (2014); A1;,
Chloride – Wikipedia,
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4152-90-3, name is (3-Chlorophenyl)methanamine, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: chlorides-buliding-blocks

General procedure: Amine (1 mmol), 2-aminothiophenol (2 mmol), BODIPY photosensitizer (0.01 mmol, 1.0 mol%), and acetonitrile (5 mL) were added to a dry 10-mL flask. The flask was pressurized with air (2 bar) and then heated to 50 C. The solution was then irradiated using a 35-W xenon lamp through a cutoff filter (0.72M NaNO2 aqueous solution, which is transparent for light >385nm, because lamps could emit a small amount of ultraviolet light). After the reaction was completed, the solvent was evaporated under reduced pressure. The crude product was further purified using column chromatography.

The synthetic route of 4152-90-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhou, Zeyin; Yang, Weijun; Synthetic Communications; vol. 44; 21; (2014); p. 3189 – 3198;,
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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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine

To a solution of 2,4-dichloropyrrolo[2,l-f [l,2,4]triazine (la) (3 g, 15.96 mmol, CASNo. 918538-05-3) in DMF (50 mL) under Ar atmosphere was added 1 -ethoxy vi nyltri -//-butylti n (7.07 mL, 20.74 mmol, CASNo. 97674-02-7) and bis(triphenylphosphine)Palladium(II)chloride (0.56 g, 0.8 mmol). The mixture was heated with stirring at 100 C for 30 min, cooled to room temp and diluted with EtOAc (150 mL). The reaction mixture was washed with water (50 mL), brine (30 mL), dried, filtered and concentrated in vacuum to dryness. The residue obtained was purified by flash column chromatography [silica (24 g), eluting with EtOAc in hexane from 0-50%] to afford 2-chl oro-4-(l -ethoxy vinyl)pyrrolo[2, l-f][l, 2, 4]triazine (lb) (2.2 g, 62 % yield) as an orange oil; NMR (300 MHz, DMSO-7e) d 8.23 (dd, J= 2.6, 1.4 Hz, 1H), 7.34 (dd, J= 4.7, 1.4 Hz, 1H), 7.11 (dd, j= 4.7, 2.6 Hz, 1H), 5.64 (d, 7= 2.4 Hz, 1H), 4.88 (d, J= 2.4 Hz, 1H), 4.03 (q, J= 7.0 Hz, 2H), 1.44 (t, J= 7.0 Hz, 3H).

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 918538-05-3.

Reference:
Patent; BIOCRYST PHARMACEUTICALS, INC.; KOTIAN, Pravin, L.; BABU, Yarlagadda; ZHANG, Weihe; LU, Pen-Cheng; WU, Minwan; LV, Wei; NGUYEN, Trung, Xuan; DANG, Zhao; CHINTAREDDY, Venkat, R.; KUMAR, V., Satish; RAMAN, Krishnan; (1223 pag.)WO2019/195720; (2019); A1;,
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