Month: May 2021

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 69411-05-8, name is 3-Chloro-5-trifluoromethylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Chloro-5-trifluoromethylaniline

To a solution of 3-Chloro-5-trifluoromethyl-aniline (425 mul, 3.1 mmol, 1.03 eq.) in dry THF (15 ml) was added 4-Chloro-3-(trifluoromethyl)-phenylisocyanate (665 mg, 3.0 mmol). After stirring overnight at rt the mixture was diluted with cHexane (100 ml), washed twice with 2 N HCl, once with sat. NaHCO3 and brine (100 ml each) and adsorbed on Celite in vacuo. Flash chromatography on silica with cHexane/TBME (4:1 to 2:1) yielded 952 mg product (76%) as a white powder. 1H NMR (DMSO) delta 9.43 (s, 2H), 8.10 (d, J=2.5 Hz, 1H), 7.84 (m, 2H), 7.69 (dd, J=9.0, 2.5 Hz, 1H), 7.64 (d, J=9.0 Hz, 1H), 7.45 (s). MS (ES-): 414.9.

The synthetic route of 69411-05-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Arpida AG; US2009/23813; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1009102-44-6, 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 1009102-44-6 as follows.

To a solution of (E)-3-((3aS,5aR,5bR,7aR,9S,11aR,11bR,13aS)-9-hydroxy-1- isopropyl-5a,5b,8,8, 11 a-pentamethyl-2-oxo- 3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a, 11b, 12,13, 13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)-2-methylacrylic acid (350 mg, 0.685 mmol), 1-(4- chlorophenyl)cyclopropanamine hydrochloride (154 mg, 0.754 mmol) and HATU (521 mg, 1.371 mmol) in DMF (2 mL) stirred at 0C was added DIPEA (0.479 ml_, 2.74 mmol). The reaction mixture was stirred at 20C for 1h. The reaction mixture was pH adjusted to 3-4 with 2 M HCI and filtered. The solid was washed with water (50 mL), dissolved into DCM, dried over sodium sulfate and evaporated in vacuo to give the crude (E)-N-(1-(4- chlorophenyl)cyclopropyl)-3-((3aS,5aR,5bR,7aR,9S, 11 aR, 11 bR, 13aS)-9-hydroxy-1 – isopropyl-5a,5b,8,8, 11 a-pentamethyl-2-oxo- 3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a, 11b, 12,13, 13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)-2-methylacrylamide (650 mg, 0.680 mmol, 99 %) as a yellow solid.

According to the analysis of related databases, 1009102-44-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXOSMITHKLINE LLC; HAN, Nianhe; JOHNS, Brian Alvin; TANG, Jun; WO2013/90683; (2013); 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. 454-78-4, name is 2-Bromo-1-chloro-4-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Computed Properties of C7H3BrClF3

Preparation of [2-chloro-5-(trifluoromethyl)phenyl]-(2,6-difluorophenyl)methanone (3a); Anhydrous LiCl (16 mol) is introduced in a 25 ml-Schlenk flask having been rinsed with argon and dried under high vacuum (<1 mbar) at 150-170 C. for 5 minutes. Zinc powder (15 mmol) is added under argon and the flask is three-times evacuated and filled with argon. Then, dry THF (10 ml) is added and the zinc is activated with BrCH2CH2Br (5 mol %) and Me3SiCl (1 mol %). The mixture is heated to 50 C. and then, 2-bromo-1-chloro-4-(trifluoromethyl)benzene (5 mmol) in 2 ml dry THF with an internal standard (n-tetradecane) of about 10% are added, followed by 5 mmol N,N,N',N',N-pentamethyldiethylenetetramine. The insertion reaction is completed after 15 hours (control by use of an GC analysis of reaction aliquots wherein the reaction has proceeded for more than 99%). The solution of bromo-[2-chloro-5-(trifluoromethyl)phenyl] zinc (2.5 mmol, 5.5 ml) is carefully separated from the remaining zinc powder by use of a syringe and transferred into another 10 ml-Schlenk flask having been rinsed with argon. The synthetic route of 454-78-4 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Knochel, Paul; Gavryushin, Andrei; Malakhov, Vladimir; Krasovskiy, Arkady; US2011/84230; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 202865-57-4, A common heterocyclic compound, 202865-57-4, name is 1-Bromo-2,5-dichloro-3-fluorobenzene, molecular formula is C6H2BrCl2F, 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.

Preparation 19 1-Bromo-2,5-dichloro-3-methoxybenzene 1-Bromo-2,5-dichloro-3-fluorobenzene (40 g, 0.16 mol) and sodium methoxide (44.3 g, 0.82 mol) were stirred in methanol (500 ml) at the reflux temperature for 16 hours. The reaction was cooled to ambient temperature then quenched with water (500 ml). The mixture was extracted with diethyl ether (3*300 ml), dried (Na2SO4) and evaporated to afford the product as a white solid (40 g) 1H-NMR (CDCl3): 3.90 (s, 3H), 6.86 (d, 1H), 7.26 (d, 1H). MS m/z 256 [MH]+ GC-MS m/z 256 [MH]+, Rt=4.58 min

The synthetic route of 202865-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Limited; US2007/105872; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 22911-21-3, A common heterocyclic compound, 22911-21-3, name is 1-Chloro-4-(trimethoxymethyl)benzene, molecular formula is C10H13ClO3, 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.

1-Chloroisoquinolin-5-amine A mixture of 1-chloro-5-nitroisoquinoline (450 mg, 0.0022 mol), stannous chloride dihydrate (2.4 g, 0.011 mol), and EtOAc (50 mL) was stirred under reflux under an atmosphere of nitrogen for 3 h. After cooling, the mixture was poured into ice-water and basified to pH 10.0 with aq. Na2CO3. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated under vacuum. The residue was purified by column chromatography on silica gel to give the product as a light yellow solid. LC-MS: 3.17 min, 179.2 & 181.2 (M+1).

The synthetic route of 22911-21-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kelly, Michael G.; Kincaid, John; Duncton, Matthew; Sahasrabudhe, Kiran; Janagani, Satyanarayana; Upasani, Ravindra B.; Wu, Guoxian; Fang, Yunfeng; Wei, Zhi-Liang; US2006/194801; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 33353-68-3,Some common heterocyclic compound, 33353-68-3, name is 3,5-Dichloro-2-methoxyaniline, molecular formula is C7H7Cl2NO, 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.

6,8-Dichloro-5-methoxy-2H-benzorein ,2,41thiadiazin-3(4H)-one 1 ,1 -dioxide (lnt-24) A 250 mL round-bottomed flask was charged with chlorosulfonyl isocyanate (0.717 ml) in nitropropane (40 ml) to give a colorless solution at -40 C under nitrogen. After 10 min, a solution of 3,5-dichloro-2-methoxyaniline (1220 mg) in nitropropane (20 ml) was added to the reaction mixture. After 10 min, the reaction was warmed to 0 C. After 30 min, aluminum chloride (1 101 mg) was added to the reaction mixture. After 5 min, the reaction mixture was warmed to 100 C. After 45 min, the reaction mixture was poured in ice/water (400 mL) and stirred for 1 h. The solids were filtered and washed with water and hexanes, and dried in a vacuum oven overnight to obtain the titled compound (391 mg). LCMS m/z 297.1 (M+H).

The synthetic route of 33353-68-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ADAMS, Jerry Leroy; ATOR, Laura E.; DUFFY, Kevin J.; GRAYBILL, Todd L.; KIESOW, Terence John; LIAN, Yiqian; MOORE, Michael Lee; RALPH, Jeffrey M.; RIDGERS, Lance Howard; (370 pag.)WO2017/98421; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 621-62-5, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 621-62-5, name is 2-Chloro-1,1-diethoxyethane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 4-bromo-6-chloropyridazin-3-amine (15.7 g, 75.3 mmol), 2-chloro-1,1-diethoxyethane (13.9 g, 90.3 mmol) and PTSA (17.2 g, 90.3 mmol) in isopropanol (150 mL) was heated to 80 C. for 20 h. After cooling to room temperature, the solution was concentrated in vacuo. The resulting mixture was treated with a saturated NaHCO3 solution (300 mL), extracted with dichloromethane (200 mL×3), dried over Na2SO4, filtered and concentrated. The residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=3:1) to give 8-bromo-6-chloroimidazo[1,2-b]pyridazine (17.2 g, 98%) as an orange solid. LC-MS: [M+H]+, 231.9, 233.9, tR=1.46 min.

The synthetic route of 2-Chloro-1,1-diethoxyethane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; Hermann, Johannes Cornelius; Kuglstatter, Andreas; Lucas, Matthew C.; Padilla, Fernando; Wanner, Jutta; Zhang, Xiaohu; US2013/109661; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 54730-35-7, These common heterocyclic compound, 54730-35-7, name is 3,5-Dichloro-4-methylaniline, 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.

Preparation 2; 5-bromo- 1 ,3-dichloro-2-methylbenzene; Suspend the 3,5-dichloro-4-methylaniline in 48percent HBr (5 mL) and water (5 mL) and heat with a heat gun until the mixture is near the boiling point. Cool the slurry to room temperature and then cool to 00C with an ice/brine bath. Add a solution of sodium nitrite (109 mg, 1.58 mmol) in water (2 mL) dropwise. After the addition is complete, stir the reaction an additional 15 min in the cold bath. Add a solution of CuBr (1.08 g, 7.53 mmol) in 48percent HBr (2 mL) and heat the rapidly stirring reaction to 500C for 1 hour. Cool the reaction to room temperature, dilute the reaction with ethyl acetate and discard the aqueous layer. Wash the organic layer with water and brine, dry with MgSO4, filter through celite and concentrate to an orange residue. Purify the residue by silica gel chromatography eluting with hexanes to afford 164 mg (45percent) of the product as a yellow solid.

The synthetic route of 54730-35-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2007/127763; (2007); A2;,
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. 320-60-5, name is 2,4-Dichloro-1-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., SDS of cas: 320-60-5

Example 3; R-(+)-[2-(2,4-Dichloro-phenyl)-2-(4-fluoro-phenyl)-6-fluoro-benzo[1,3]dioxol-5-yl]-morpholin-4-yl-methanone; Preparation of 2,4-dichloro-4′-fluoro-diphenyldichloromethane; To a cooled (0 C.) suspension of aluminium trichloride (2.02 g, 15 mmol, 3.0 eq.) in 1,2-dichloroethane (7 mL) was slowly added 2,4-dichlorobenzotrifluoride (1.1 g, 5 mmol) followed by fluorobenzene (0.483 g, 5 mmol, 1.0 eq.). The reaction mixture was stirred at 0-5 C. for 5 h, then poured onto ice and extracted with dichloromethane. The combined organic layer was washed with brine, dried over sodium sulfate and filtered. The volatiles were removed in vacuo, affording the title compound (1.63 g, quant.) as yellow oil. MS: m/e=325.0 ([M+H]+).

The synthetic route of 320-60-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Frei, Beat; Plancher, Jean-Marc; Roever, Stephan; Zimmerli, Daniel; US2006/293318; (2006); 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. 21402-26-6, name is 4-Bromo-3-chloroaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H5BrClN

EXAMPLE 53 9-(Trifluoromethyl)-1,2,3,6-tetrahydro-7H-[1,4]thiazino[3,2-g]quinolin-7-one (Compound 156, Structure 54 of Scheme XI, where R4=H) 6-Bromo-7-chloro-2-isopropoxy-4-(trifluoromethyl)quinoline (Structure 51 of Scheme XI). This compound was prepared according to General Method 11 (EXAMPLE 22) from 4-bromo-3-chloroaniline (2.06 g, 10.0 mmol), ethyl 4,4,4-trifluoroacetoacetate (2.30 g, 12.5 mmol) in 50 mL toluene followed by heating in 33 mL conc. H2SO4 to afford 2.08 g (64%) of 6-bromo-7-chloro-4-(trifluoromethyl)-quinolin-2(1H)-one, an off-white solid.

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 21402-26-6.

Reference:
Patent; Ligand Pharmaceuticals, Inc.; US6462038; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics