Month: January 2021

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. 933190-51-3, name is 8-Bromo-6-chloroimidazo[1,2-b]pyridazine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 8-Bromo-6-chloroimidazo[1,2-b]pyridazine

0O150] Step 1: To a solution of 8..bromo.-6chioroirnidazo[i,2bjpyridazine (1.0 equiv.) and diethyl 2-methylmalonate (1.0 equiv.) in DMF (0.15 M) was added sodium hydride (2.5 equiv.) at it The reaction was stined for 10 mm, then quenched with saturated ammoniurn chloride and extracted twice with ethyl acetate. The organic phase was dried with magnesium sulfate, filtered and concentrated. The residue was purified via reverse phase prep-1-IPLC to give cliethyl 2-(6-chloroimidazo[i ,2-bpyridazin-8.yI)-2-rnethylmalonate in 21% yield. LCMS (m/z) (M¡ÀH) 326.0, Rt 0.84 miii.

According to the analysis of related databases, 933190-51-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NOVARTIS AG; AVERSA, Robert John; BURGER, Matthew T.; DILLON, Michael Patrick; DINEEN JR., Thomas A.; LOU, Yan; NISHIGUCHI, Gisele A; RAMURTHY, Savithri; RICO, Alice C.; RAUNIYAR, Vivek; SENDZIK, Martin; SUBRAMANIAN, Sharadha; SETTI, Lina Quattrocchio; TAFT, Benjamin R.; TANNER, Huw Rowland; WAN, Lifeng; (307 pag.)WO2016/38582; (2016); A1;,
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These common heterocyclic compound, 67279-24-7, name is 1,4-Dichloro-5,6,7,8-tetrahydrophthalazine, 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. category: chlorides-buliding-blocks

A solution of l,4-dichloro-5,6,7,8-tetrahydro-phthalazine (CAS 67279-24-7; 348 mg, 1.7 mmol) in concentrated aqueous N (5 ml) and ethanol (5 ml) was stirred at 120C in an autoclave for 20 h. The mixture was cooled to r.t. and concentrated. The crude product was purified by silica gel chromatography using a chromatography using a CE^Ck/MeOH gradient as eluent, to provide the title compound (52 mg, 16%>) as off- white solid. MS: M = 184.2 (M+H)+

The synthetic route of 1,4-Dichloro-5,6,7,8-tetrahydrophthalazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; FLOHR, Alexander; GROEBKE ZBINDEN, Katrin; LERNER, Christian; WO2014/72261; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 2687-12-9, A common heterocyclic compound, 2687-12-9, name is Cinnamyl chloride, molecular formula is C9H9Cl, 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.

Specifically, a 200 mL flask containing 15.3 g (0.1mol) of compound lb and 25 g (0.15 mol) of triethyl phos-phite was stirred for 8 hours at 180 C.Next, afier cooling the flask to room temperature, excess triethyl phosphite was evaporated under reduced pressure to yield 22 g (percentage yield: approximately 87%) ofthe compound 3b (white liquid).

The synthetic route of 2687-12-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KYOCERA Document Solutions Inc.; OKADA, Hideki; SUGAI, Fumio; KOJIMA, Kensuke; (23 pag.)US2016/152552; (2016); 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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-(2-Chloroethyl)azepane hydrochloride

To a solution of 1,1-bis(4-hydroxyphenyl)-2,2-diphenylethene (27.2 mg, 74.6 mumol) in DMF (0.75 mL) at 0 ¡ãC was added 60percent sodium hydride (dispersion in paraffin liquid, 23.9 mg, 0.598 mmol). The reaction mixture was stirred for 15 min at 50 ¡ãC and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (48.8 mg, 0.246 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 1 h at 50 ¡ãC, saturated aqueous ammonium chloride was added at 0 ¡ãC. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 30/1) to afford RID-F-S*14 (compound 10) (37.9 mg, 83percent) as a brown oil

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 26487-67-2.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

14862-52-3, name is 3,5-Dibromochlorobenzene, 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. Formula: C6H3Br2Cl

Intermediate 1-2 (2.8 g, 0.010 mol) was added intermediate 1-3 (4.2 g, 0.011 mol),Pd (dba) 2 (0.5 g, 0.0005 mol), 100 mL of Toluene was added to sodium-tert-butoxide (1.9 g, 0.020 mol), and the mixture was reacted at 95 C. for 4 hours with stirring.After completion of the reaction, the mixture was separated into H 2 O: MC and purified by column (N-HEXANE: MC) to obtain 3.6 g (yield: 62%) of Intermediate 1-4. To 1,3-dibromo-5-chlorobenzene (2.7 g, 0.010 mol) was addedN-phenylbiphenyl-4-amine (5.4 g, 0.022 mol) was added to the reaction mixture to obtain 4.4 g (yield 73%) of Intermediate 7-1.

The synthetic route of 14862-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; P&H Tech Co.,Ltd; Hyun, Sao Yong; Jung, Sung Wook; Kim, Ha Yeon; (48 pag.)KR2016/79514; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 108-70-3, A common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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.

A 50 mL 3 neck round bottom flask was oven dried, cooled under nitrogen, and char- ged with 14.50 g of xylenes. The flask was then charged with 1,3, 5-TRICHLOROBENZENE (9.760g, 53.49 MMOL), benzophenone imine (7.620 g, 42.04 MMOL), (dba) 3PD2 CATALYST (0.023 g, 0.03 mmol in 2 g xylene), dppf ligand (0.042 g, 0.08 MMOL IN 2 G XYLENE) and sodium t-butoxid (5.550 g, 57.70 mmol). The reaction mixture was heated to reflux (136 C) for 3 hours and then cooled to room temperature. The aromatic imine intermediate was then hydrolyzed with 22 ML OF 2 N HCI (aq) at 70 C for 45 minutes. The hydrochloride salt of dichloroaniline precipitated out of solution when cooled to room temperature. The crude hydrochloride salt was collected by filtration using a buchner funnel and then washed with methyl-tert. butyl ether. The DICHLOROANALINE SALT was then added to 30 mL of METHYL-TERT. BUTYL ether and pH adjusted to 12 using 50% NaOH. The methyl-tert. butyl ether phase was collected and then stripped under va- cuum to give 3, 5-DICHLOROANILINE in 86 % yield.

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF AKTIENGESELLSCHAFT; WO2004/54961; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, 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 210532-25-5, name: 3,5-Difluorobenzene-1-sulfonyl chloride

At room temperature,2-methyl-4-carbonyl-6,7,8,9-tetrahydropyrido [1,2-a] thiophene [2,3-d] pyrimidin-3-amine hydrochlorideCompound 10 (0.31 g, 1 mmol) was dissolved in anhydrous dichloromethane (10 ml)Followed by the addition of 3,5-difluorobenzenesulfonyl chloride (0.23 g, 1.1 mmol)Triethylamine (0.12 g, 1.2 mmol) was slowly added with stirring, stirred at room temperature overnight,Reaction to the material completely disappeared,Dichloromethane, concentrated, using a 5: 1 by volume petroleum ether: ethyl acetate column chromatography gradient elution,To give compound 10f; yield: 82% as a white solid

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, 3,5-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chinese Academy Of Sciences Xinjiang Physics And Chemistry Technology Institute; A Jiaikebaier¡¤aisa; Nie Lifei; Huang Guozheng; (23 pag.)CN106749317; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 344-65-0, These common heterocyclic compound, 344-65-0, name is 1-Bromo-4-chloro-2-(trifluoromethyl)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.

General procedure: A 1,4-Dioxane solution (8 mL) of 10 (1.0 mmol), arylboronic acid 2 (1.0 equiv.), K3PO4, and Pd(PPh3)4 (5 molpercent) was heated at 75 C for 4 h. After cooling to room temperature, H2O was added and the reaction mixture was extracted with CH2Cl2. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (pure n-heptane).

Statistics shows that 1-Bromo-4-chloro-2-(trifluoromethyl)benzene is playing an increasingly important role. we look forward to future research findings about 344-65-0.

Reference:
Article; Ali, Iftikhar; Siyo, Baraa; Hassan, Zahid; Malik, Imran; Ullah, Ihsan; Ali, Asad; Nawaz, Muhammad; Iqbal, Jamshed; Patonay, Tama?s; Villinger, Alexander; Langer, Peter; Journal of Fluorine Chemistry; vol. 145; (2013); p. 18 – 34;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 13918-92-8, A common heterocyclic compound, 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, molecular formula is C6H3ClF2O2S, 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.

A mixture of 1.80 g (8.8 mmol) C-5, 2.29 mL (17 mmol) 2,4-difluorobenzenesulphonyl chloride, 1.07 mL (13.3 mmol) pyridine and 20 mL DCM is stirred at RT over night. 100 mL DCM is added and the reaction mixture is extracted three times with 50 mL aqueous 1M HCl. The organic layer is dried over MgSO4 and the solvent is removed under reduced pressure. The solid is dissolved in water/MeCN and further purified by RP-chromatograpy. Yield: 2.9 g (86%).

The synthetic route of 13918-92-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WUNBERG, Tobias; KRAEMER, Oliver; van der VEEN, Lars; US2013/23533; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 4535-90-4, These common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine 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.

A mixture of intermediate 33 (0.56 g; 1.46 mmol), tetrabutylammonium bromide (0.12 g; 0.37 mmol) and KOH (1.23 g; 21.9 mmol) in 2-methyltetrahydrofuran (8.5 mL) and water (1 mL) was heated at 50C for 1 hour. Methylaminoethyl chloride hydrochloride (0.34 g; 2.63 mmol) was added and the mixture was heated at 50C overnight. Water (200 mL) was added and the mixture was extracted with DCM (3 x 150 mL). The combined organic layers were dried over Na2S04, filtered and concentrated. The residue was purified by column chromatography over silica gel (eluent: DCM/MeOH 98/2 to 85/15). The fractions containing the product were collected and concentrated to afford after trituration in Et20 and drying under vacuum to give 0.408 g of the expected compound. This solid was purified by achiral SFC on (AMINO thetamuiotatauiota 150×21.2mm; mobile phase: 0.3% isopropylamine, 75% C02, 25% MeOH) to give 308 mg of an intermediate residue which was crystallized from Et20 to afford 256 mg (40%) of compound 30 . MP: 120C (gum) (Kofler).

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; ANGIBAUD, Patrick Rene; OBRINGER, Michel; MARIN, Julien Jeremie Joseph; JEANTY, Matthieu; WO2013/61077; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics