Chlorides-buliding-blocks

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. 766545-20-4, name is 2-Chloro-5,6,7,8-tetrahydro-1,6-naphthyridine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., category: chlorides-buliding-blocks

Following the procedure described in Example 12,Was reacted with 0.84 g (0.0075 mmol) of N-cyanoethyl ester from 1.03 g (0.005 mol) of 2-chloro-5,6,7,8-tetrahydro-1,6-naphthyridine hydrochloride,To give 0.8 g of a white solid, A mixture of 1.2 g (0.004 mol) of 2-chloro-4,5,6,7-tetrahydrothiazole [5,4-c] pyridine trifluoroacetate,0.67 g (0.006 mol)N-cyanoethyl esterWas added to a reaction flask equipped with 30 ml of methanol,0.73 g (0.0048 mol) of DBU was added,Heating to reflux reaction,After 2 hours the TLC monitoring reaction was complete,Cooling white solid precipitation,

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 766545-20-4.

Reference:
Patent; Shenyang Sinochem Pesticide Chemical Research and Development Co., Ltd.; Yang, Jichun; Li, Miao; Fan, Xiaoxi; Yang, Fan; Li, Keke; Liu, Zhangling; (46 pag.)CN106467538; (2017); A;,
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. 1939-99-7, name is Phenylmethanesulfonyl chloride, A new synthetic method of this compound is introduced below., Application In Synthesis of Phenylmethanesulfonyl chloride

To a solution of 2-((tert-butyldimethylsilyl)oxy)ethanamine (11.7 g, 66.6 mmol) and triethylamine (11.2 mL, 79.9 mmol) in tetrahydrofuran (222 mL) at 0 C. was slowly added phenylmethanesulfonyl chloride (12.7 g, 66.6 mmol) portion wise and the reaction was stirred at room temperature for 16 hours. MTBE was then added and the Et3N.HCl salt was removed by filtration. The filtrate was then concentrated and purified by silica gel solumn chromatography (0-30% Acetone in heptane, 216 nM) to N-(2-((tert-butyldimethylsilyl)oxy)ethyl)-1-phenylmethanesulfonamide (17.8 g, 81% yield). LCMS (ESI), m/z, 330. [M+H]+.

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

Reference:
Patent; Genentech, Inc.; Fauber, Benjamin; Gobbi, Alberto; Rene, Olivier; van Niel, Monique Bodil; Gancia, Emanuela; Gaines, Simon; Ladduwahetty, Tammy; Vesey, David; Ward, Stuart; Winship, Paul; (101 pag.)US2016/168141; (2016); 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. 1205-71-6, name is 4-Chloro-N-phenylaniline, A new synthetic method of this compound is introduced below., Formula: C12H10ClN

General procedure: 0.248 g (1.00 mmol) of (4-bromophenyl) phenylamine, 0.176 g (1.05 mmol) of 9H-carbazole,4.6 mg (5.0 mumol) of tris (dibenzylideneacetone) dipalladium,14.9 mg (35.0 mumol) of 2- (di-tert-butylphosphino) -2 ‘, 4′, 6′-triisopropyl-1,1’-biphenyl,After 0.144 g (1.50 mmol) of sodium tert-butoxide and 3 mL of o-xylene were added, the inside of the reaction system was replaced with argon gas.Thereafter, the mixture was heated to 140 C. and stirred for 15 hours. After cooling to room temperature, the reaction was stopped by adding 25 mL of water. Further, 20 mL of ethyl acetate and 9- (p-tolyl) -9H-carbazole as an internal standard were added and stirred until the ethyl acetate layer became homogeneous.The ethyl acetate layer (0.2 mL) was collected, diluted with tetrahydrofuran 4 mL, and the conversion of (4-bromophenyl) phenylamine was 99% or more by HPLC analysis,It was confirmed that 98% of 9- [4- (phenylamino) phenyl] -9H-carbazole was formed relative to (4-bromophenyl) phenylamine.

The synthetic route of 1205-71-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SAGAMI CHEMICAL RESEARCH INSTITUTE; TOSOH CORPORATION; YAMAKAWA, TETSU; OHTSUKA, YUKI; MIYAZAKI, TAKANORI; (28 pag.)JP2018/90563; (2018); A;,
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. 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Product Details of 7051-16-3

General procedure: To a solution of 4-bromoanisole (200.8 mg, 1.09 mmol, 1.0 equiv) in acetonitrile (2 mL) was added N-chlorosuccinimide(NCS) (158.3 mg, 1.19 mmol, 1.1 equiv) at rt to give a slightly cloudy mixture. Chlorotrimethylsilane (TMSCl) (14 muL, 0.11 mmol, 0.1 equiv) was then added drop-wise to the reaction mixture. Within a few minutes, the reaction mixture became clear pale yellow solution. The mixture continued to stir at rt for 1 h and was diluted with hexane. The biphasic mixture was concentrated on a rotary evaporator to a crude white solid-oil mixture. This mixture was taken up in hexane and filtered through a short plug of SiO2 and eluted with 5-10% EtOAc-hexane solution. The clear filtrate was concentrated to obtain a mixture of 4-bromo-2-chloro-1-methoxybenzene (2a-Cl) and 2,4-dichloro-1-methoxybenzene (2a-diCl) 237.0 mg (88% of 2a-Cl and 11% of 2a-diCl,based on NMR ratio 2a-Cl: 2a-diCl = 7.1: 1.0; as a pale yellow solid).

The synthetic route of 7051-16-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Maibunkaew, Tapanee; Thongsornkleeb, Charnsak; Tummatorn, Jumreang; Bunrit, Anon; Ruchirawat, Somsak; Synlett; vol. 25; 12; (2014); p. 1769 – 1775;,
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. 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 104-11-0

General procedure: A solution of 0.17g (1.40mmol) of N-benzylmethylamine, 0.20g (1.40mmol) of K2CO3 and 0.40g of (R,S)-3(4-bromobutyl)-5-phenyloxazolidin-2-one 23 in ACN was allowed to stirring under reflux for 6-12h and monitored by TLC until the reaction was completed. The hot solution was filtered and concentrated in vacuo to afford 0.29g (85.0mmol) of a chromatography pure yellow oil 2a.

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 104-11-0.

Reference:
Article; Zampieri, Daniele; Vio, Luciano; Fermeglia, Maurizio; Pricl, Sabrina; Wuensch, Bernhard; Schepmann, Dirk; Romano, Maurizio; Mamolo, Maria Grazia; Laurini, Erik; European Journal of Medicinal Chemistry; vol. 121; (2016); p. 712 – 726;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 626-43-7, A common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, molecular formula is C6H5Cl2N, 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.

To a solution of 3,5-dichloroaniline (3.56 g, 21.97 mmol) in acetonitrile (60 mL) at 0C was added NBS (4.30 g, 24.17 mmol). The reaction was kept at 0C and stirred for 3 h. The solvent was concentrated under reduced pressure and the residue was partitioned between EtOAc (200 mL) and water (100 mL). The organic layer was washed with brine, dried over MgS04, filtered and concentrated in vacuo. The residue was purified by chromatography on silica (Eluant: Hexane:EtOAc = 90: 10) to afford the title compound 4-bromo-3,5-dichloroaniline. LCMS calc. = 239.89; found = 239.84/241.84 (M+H)+. NMR (500 MHz, CDC13): delta 7.71 (s, 2 H); 3.80-

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; MERCK SHARP & DOHME CORP.; MOCHIDA PHARMACEUTICAL CO., LTD.; ZHANG, Ting; CHEN, Yi-Heng; GUO, Liangqin; HRUZA, Alan; JIAN, Tianying; LI, Bing; MENG, Dongfang; PARKER, Dann, L., Jr.; SHERER, Edward, C.; WOOD, Harold, B.; SAKURADA, Isao; (130 pag.)WO2016/94260; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 101-79-1,Some common heterocyclic compound, 101-79-1, name is 4-(4-Chlorophenoxy)aniline, molecular formula is C12H10ClNO, 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. r4- (4-Chloro-phenoxy)-phenylaminol-acetic acid ethyl ester. Oxo-acetic acid ethyl ester (0.243 g, 2.38 mmol) was added to a solution of 4- (4-chloro- phenoxy)-phenylamine (0.5 g, 2.27 mmol) in DCE (48 mL). The mixture was stirred at rt for 15-20 min, before the addition of Na (OAc) 3BH (0.625 g, 2.95 mmol) and AcOH (0.24 mL). The mixture was stirred at rt for 5 h. More oxo- acetic acid ethyl ester (0.08 g) and AcOH (0.03 mL) were added, and the mixture was stirred at rt overnight. Saturated NaHCO3 (50 mL) and excess CH2CI2 (50 mL) were then added to the reaction mixture. The aqueous layer was extracted with CH2CI2 (3 X 50 mL). The combined organic layers were washed with brine (40 mL) and dried (MgS04), and the solvent was removed. Purification by column chromatography with 20-50percent EtOAc/hexanes afforded 0.4 g (61 percent) of the desired product. MS (electrospray) : mass calculated for Ct4H12CINO3, 305.76 ; m/z found, 306.1 [M+H] +.’H NMR (400 MHz, CDCI3) : 7.25-7. 23 (m, 2H), 6.93-6. 86 (m, 4H), 6.64-6. 62 (m, 2H), 4.28 (dd, J= 14.3, 7.1 Hz, 2H), 3.92 (s, 2H), 1.33 (t, J= 7.1 Hz, 3H).

The synthetic route of 101-79-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA, N.V.; WO2005/44810; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 1127-85-1, A common heterocyclic compound, 1127-85-1, name is 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, molecular formula is C8H8Cl2N2, 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.

Step C: Synthesis of (2-chloro-5,6,7,8-tetrahydro-quinazolin-4-yl)-methyl-amine. To a solution of 2,4-dichloro-5,6,7,8-tetrahydro-quinazolin (8.70 g, 42.8 mmol) in THF (87 mL) was added 40% aqueous MeNH2 (8.32 g, 107 mmol). The mixture was stirred at ambient temperature for 8 hr. The solution was poured into saturated aqueous NaHCO3 and the aqueous layer was extracted with CHCl3 (three times). The combined organic layer was dried over MgSO4, filtrated, concentrated, and purified by flash chromatography (NH-silica, 50% EtOAc in hexane) to give (2-chloro-5,6,7,8-tetrahydro-quinazolin-4-yl)-methyl-amine (7.04 g, 83%) as a white solid. ESI MS m/e 220, M + Na+; 1H NMR (300 MHz, CDCl3) delta 1.74-1.92 (m, 4 H), 2.26 (t, J= 5.5 Hz, 2 H), 2.67 (t, J= 5.6 Hz, 2 H), 3.05 (d, J= 5.0 Hz, 3 H), 4.81 (s, 1 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; Taisho Pharmaceutical Co. Ltd.; Arena Pharmaceuticals, Inc.; EP1464335; (2004); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 367-22-6, 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. 367-22-6 name is 4-Chloro-3-fluoroaniline, 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.

At 0 C, to a mixture of 4-chloro-3-fluoroaniline (7 g, 48.1 mmol) in DCM (100 mL) was added pyridine (7.8 mL, 96 mmol), followed by phenyl carbonochloridate (6.3 mL, 50.5 mmol). The mixture was stirred at 0 C for 1 h, then warmed up to rt overnight. The mixture was washed with IN HCl and back extracted with DCM. The combined organics were washed with brine, dried over anhydrous Na2SO4, and filtered. The filtrate was concentrated to give phenyl (4-chloro-3-fluorophenyl)carbamate (12 g, 45.2 mmol, 94 % yield) as a colorless solid. The crude product was used without further purification.LC/MS (ESI): m/z 266.1 (M+H)+, 1.13 min (ret. time).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-3-fluoroaniline, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BAILEY, James; CHEN, Yao; HURLE, Mark; LEACH, Craig; TURUNEN, Brandon; (103 pag.)WO2018/134731; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 6940-78-9,Some common heterocyclic compound, 6940-78-9, name is 1-Bromo-4-chlorobutane, molecular formula is C4H8BrCl, 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.

Preparation of 4-Methyl-l,2,4-triazine-3,5(2H,4H)-dione2-Acetyl-l,2,4-triazine-3,5(2H,4H)-dione (10 g, 64.5 mmol) was added portionwise over 40 min to a suspension of sodium hydride (3.09 g, 60wt suspension in oil, 77.4 mmol) in DMF (160 mL) and stirred vigorously for 45 min. Iodomethane (4.41 mL, 10.1 g, 70.9 mmol) was added and the whole mixture stirred at ambient temperature for 66 h under a dry nitrogen atmosphere. A slight ppt remained but this disappeared on warming to evaporate the solvent. The residue was dissolved in EtOH (200 mL) and /rara-toluenesulfonic acid monohydrate (1.4 g, -10 mol ) was added and the yellow solution refluxed for 2 h before allowing to cool. Solvent was evaporated and toluene (275 mL) added with heating. After standing overnight, solid was filtered off. The crude solid was suspended in EtOAc (250 mL) and stirred overnight to dissolve out sodium iodide, then filtered off to give 4-methyl-l,2,4-triazine-3,5(2H,4H)-dione (4.9 g, 60%).1H NMR (300 MHz, DMSO-d6) 5 3.10 (3H, s, CH3), and 7.48 (lH, s, CH). 13C NMR (75 MHz, DMSO-d6) delta 25.6 (CH3), 134.4 (CH), 149.4 (NHC(=0)CH), and 156.5 (NHC(=0)NH).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-4-chlorobutane, its application will become more common.

Reference:
Patent; GE HEALTHCARE LIMITED; MEDI-PHYSICS, INC.; NEWINGTON, Ian, Martin; WYNN, Duncan George; NAIRNE, Robert James Domett; GUILBERT, Benedicte; MANDAL, Subrata; JINTO, Jose; VARADARAJAN, Sunderaraman; RANGASWAMY, Chitralekha; BETTS, Helen; DAVIS, Rebecca; WO2011/150183; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics