Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, COA of Formula: C3H4Cl3NO

EXAMPLE 2 The preparation of a mixture of 1,1′-bis(tridecyloxycarbonyl)-dimethyl-2,2′-bibenzimidazoles in which each benzene ring contains a methyl group in the 5- or 6-position. 3,4-Diaminotoluene (100.8 g) was dissolved in methanol (600 cm3) at room temperature. The solution was stirred while methyl 2,2,2-trichloroacetimidate (70.6 g) was added in a manner similar to that described in Example 1. The mixture was allowed to cool and was stirred at room temperature for 36 hours, then diluted with water (1.5 dm3) and filtered. The solid was added again to water (1 dm3) stirred at room temperature and filtered. The solid was added to aqueous 2N sodium carbonate solution (1 dm3) stirred at 70 C. for 12 hours, cooled and filtered. The solid was repeatedly washed with methanol (3*500 cm3) by slurrying and filtering to leave a pale tan coloured solid. This solid was treated with activated carbon, recrystallized from boiling dimethylformamide, and dried, yielding 49 g of 5,5′-dimethyl-2,2′-bibenzimidazole. By this method the free base rather than the monohydrochloride was isolated (found Cl<0.2%). The structure was confirmed by measurement of the proton NMR spectrum using a solution in trifluoracetic acid with tetramethylsilane as internal standard. 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, Methyl 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see. Reference:
Patent; Imperial Chemical Industries PLC; US5258524; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2163-00-0, These common heterocyclic compound, 2163-00-0, name is 1,6-Dichlorohexane, 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.

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%¡Á0.95¡Á1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%¡Á0.94¡Á1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); 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. 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 4535-90-4

A mixture of 2-t-butylaniline (5.4 g) andmethylchlorethylamine hydrochloride (7 g) and K2C03 (5 g) inNal (2 g) in diglyme (150 m) was heated at 170 2C for 8 h.The reaction was filtered and the filtrate was evaporatedunder high vacuum. The residue was mixed with EtOAc (200 ml)and H20 (200 ml) and extracted with EtOAc twice. Thecombined organic layer was washed with brine and dried overNa2S04 and evaporated to give crude 1-[2-(tert-butylphenyl]-4-methylpiperazine. The crude 1-[2-(tert-butylphenyl]-4-methylpiperazine (260 mg) was stirred with H2S04 (3 ml) atOaC and HN03 (1.2 ml, 70%) was slowly added to the reaction.The reaction was warmed to RT, stirred for 30 min, poured onice and basified with K2C03 slowly. The solution wasextracted with EtOAc three times, washed with H20, followedby brine, dried over Na2S04 and evaporated under reducedpressure. The residue was purified by column chromatographyto give 1-[2-(tert-butyl)-5-nitrophenyl]-4-methylpiperazine(260 mg) , which was hydrogenated under H2 atmosphere to give1-[2-(tert-butyl)-5-aminophenyl]-4-methylpiperazine.

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 4535-90-4.

Reference:
Patent; AMGEN INC.; WO2006/12374; (2006); 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 75717-77-0 as follows. Product Details of 75717-77-0

General procedure: A solution of 3-azido-1-tert-butyl-3-nitro-azetidine 5 (995 mg, 5 mmol) and substituted acetylene (c-k) (5.25 mmol.) in THF (40 ml) was treated at room temperature by adding a solution of ascorbic acid (440 mg, 2.5 mmol) in water (20 ml), followed by a solution of CuSO4¡¤5H2O (188 mg, 0.75 mmol) in water (10 ml). The reaction mixture was stirred for 2-6 h at room temperature. After the reaction was complete according to TLC, the mixture was diluted with water (20 ml) and extracted with CH2Cl2 (4¡Á20 ml). The organic layer was dried over Na2SO4, the solvent was removed at reduced pressure, and the residue was purified by flash chromatography (EtOAc/n-hexane, 2:3) to give the desired products 6c-k as colorless solids.

According to the analysis of related databases, 75717-77-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Dubovis, Mikhail V.; Rudakov, Gennady F.; Kulagin, Alexander S.; Tsarkova, Kseniya V.; Popkov, Sergey V.; Goloveshkin, Alexander S.; Cherkaev, Georgiy V.; Tetrahedron; vol. 74; 6; (2018); p. 672 – 683;,
Chloride – Wikipedia,
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Electric Literature of 106131-61-7,Some common heterocyclic compound, 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, molecular formula is C2Cl2N4, 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.

1,2,4-Triazole (3:5 g 50 mmol) was dissolved in 200 mL acetone, and 20 mL (12 mmol) of a 0:6M solution of 3,6-dichloro-tetrazine in acetonitrile was added. The solution was refluxed for 20 h. After cooling the resulting precipitate was washed with water and acetone. 2:1 g (9:9 mmol,83%) of (7) was isolated as an orange powder. – Elemental analysis (C6H4N10, 212.21) exp. (calcd.) in %: C33.43 (33.34), N 64.33 (64.80), H 1.87 (1.87). – DSC(5 C min1): Tdec:: 245 C (onset). – 1H NMR ([D6]DMSO,25 C, ppm): d =8.34 (s, 1H, C-H), 9.46 (s, 1H, C-H). -13C NMR ([D6]DMSO, 25 C, ppm): d =144.9 (1C), 147.2(1C), 154.2 (1C). – MS ((+)-DEI): m=z=216 [M]+ (50), 94(100), 67 (92). – Raman: n (cm-1)= 3139 (8), 3124 (12),1912 (2), 1557 (2), 1511 (63), 1483 (100), 1426 (4), 1379(21), 1336 (2), 1293 (2), 1264 (12), 1135 (19), 980 (43), 947(5), 813 (20), 662 (2). – IR (25 C, ATR): n (cm-1) = 3135(w), 3120 (w), 1813 (vw), 1755 (vw), 1551 (vw), 1514 (s),1480 (vs), 1384 (m), 1365 (m), 1337 (w), 1293 (vs), 1266 (m), 1196 (s), 1170 (vw), 1155 (s), 1116 (s), 1112 (s), 1054(s), 976 (vs), 953 (m), 939 (m), 910 (m), 880 (m), 672 (vs).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,6-Dichloro-1,2,4,5-tetrazine, its application will become more common.

Reference:
Article; Klapoetke, Thomas M.; Preimesser, Andreas; Stierstorfer, Joerg; Zeitschrift fur Naturforschung, B: Chemical Sciences; vol. 68; 12; (2013); p. 1310 – 1320;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 918538-05-3,Some common heterocyclic compound, 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, molecular formula is C6H3Cl2N3, 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.

191A. 2-Chloro-N-(5-cyclobutyl-1H-pyrazol-3-yl)pyrrolo[1,2-f][1,2,4]triazin-4-amine 5-Cyclobutyl-1H-pyrazol-3-amine (see J. Med. Chem., 2001, 44(26), 4628-4660) (89 mg, 0.65 mmol) is dissolved in isopropyl alcohol (2-3 mL), N,N-diisopropylethylamine (174 muL, 1.0 mmol) is then added, followed by the compound from 1B (85 mg, 0.45 mmol). The reaction mixture is then stirred at RT for 22 h and the solid precipitate is collected by filtration, washed with a few mL of cold isopropyl alcohol, and dried in vacuo to give 106 mg (81.5%) of the title compound as a solid: MS: 289, 291 (M+H)+, LC/MS ret. t=2.02 min.; HPLC (Method D) ret. time 15.35 min.

The synthetic route of 918538-05-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2008/9497; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 6276-54-6, The chemical industry reduces the impact on the environment during synthesis 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, I believe this compound will play a more active role in future production and life.

3-Chloropropylamine hydrochloride (1.85g, 14.2mmol) is suspended in toluene (20mL). 1.0mL of 37w% formaldehyde solution (13.4mmol) is added, then once the solids have dissolved KOH (930mg, 14.1mmol based on 85% purity) is also added. The mixture is stirred for 5h. The clear toluene phase is taken from the white paste and filtered through MgSO4. The solids are extracted with a further 1mL of toluene. The combined solutions are pumped down and the residue is dried under high vacuum for 1hr to leave a colourless oil (1.298g, 4.1mmol, 93%) which turns cloudy within a few hours. 1H NMR (m-PhF set to 7.072): delta=3.39 (6H, t, J=6.4, -CH2Cl), 3.12 (6H, s, NCH2N), 2.38 (6H, t, J=6.6, TACCH2-), 1.64 (6H, quintet, J=6.5, -CH2CH2Cl). 13C NMR – 1H-coupled, (m-PhF set to 130.476): delta=74.6 (t of quintets, J=143/4.6, NCH2N), 49.6 (t, J=133, TAC-CH2-), 43.3 (t of quintets, J=151/4.2, -CH2Cl), 31.1 (t of t, J=128/2.8, -CH2CH2Cl).

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-Chloropropan-1-amine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Koehn, Randolf D.; Coxon, Alexander G.N.; Hawkins, Christopher R.; Smith, David; Mihan, Shahram; Schuhen, Katrin; Schiendorfer, Michael; Kociok-Koehn, Gabriele; Polyhedron; vol. 84; (2014); p. 3 – 13;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, 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. HPLC of Formula: C6H3Cl2N3

116A. Preparation of 7-bromo-2,4-dichloropyrrolo[1,2-f][1,2,4]triazine A slurry of N-bromosuccinimide (4.17 g, 23.40 mmol) in 10 mL of acetonitrile was added to a cooled (0 C.) solution of 2,4-dichloropyrrolo[1,2-f][1,2,4]triazine (4 g, 21.27 mmol) in acetonitrile over 1 h. The reaction mixture was allowed to come to room temperature and stirred for an additional 16 hr to get a solution. The solvents were evaporated to get a solid. To this residue was added dichloromethane to dissolve most of the solids and the resulting solution was loaded onto 250 gm of silica in a 350 mL coarse frit funnel (preequilibrated with 5% EtOAc in hexanes). The silica gel was washed with 5% to 50% EtOAC in hexanes. The fractions were collected and evaporated to obtain 7-bromo-2,4-dichloropyrrolo[1,2-f][1,2,4]triazine (5.29 g, 93% pure) as crystals contaminated with ~7% of the 5-bromo isomer. The mixture as such was carried to the next step without further purification. MS (ESI) m/z 266.08 (M+H).

The synthetic route of 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2008/45496; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, 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 106131-61-7, COA of Formula: C2Cl2N4

General procedure: In a 100 mL round bottom flask, was introduced the diol(0.66 mmol), s-collidine (0.79 mmol) and 20 mL of dry dichloromethane and the mixture was stirred at room temperature. 3,6-dichloro-s-tetrazine 1 (0.66 mmol) was dissolved in dry dichloromethane and added dropwise in the flask. After 2 h the reaction is complete (TLC) and the solvent was removed under reduced pressure. The crude residue was purified by column chromatography on silica gel (eluent from petroleum ether/ethyl acetate 7/3 to pure ethyl acetate).

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, 3,6-Dichloro-1,2,4,5-tetrazine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Guermazi, Refka; Royer, Lorna; Galmiche, Laurent; Clavier, Gilles; Audebert, Pierre; Hedhli, Ahmed; Journal of Fluorescence; vol. 26; 4; (2016); p. 1349 – 1356;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 363-51-9, These common heterocyclic compound, 363-51-9, name is 2-Chloro-6-fluoroaniline, 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 2-chloro-6-fluoroaniline (1.5 g, 10.3 mmol), pyridine (1.0 mL, 12.4 mmol), and isobutyric anhydride (2.0 mL, 12.1 mmol) was purged with nitrogen and irradiated in a microwave reactor at 150 C. for 2 hrs. After cooling to r.t., water was added and the mixture was stirred until a solid precipitate formed. The resulting solid was then collected by filtration, washed with water, and air dried to afford N-(2-chloro-6-fluorophenyl)isobutyramide in quantitative yield as an off-white solid. The crude product obtained was used directly in the next step without further purification. LCMS calculated for C10H12ClFNO (M+H)-: m/z=216.1; Found 216.1.

Statistics shows that 2-Chloro-6-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 363-51-9.

Reference:
Patent; Incyte Corporation; Hummel, Joshua; Vechorkin, Oleg; Sokolsky, Alexander; Ye, Qinda; Liu, Kai; Yao, Wenqing; (60 pag.)US2020/48241; (2020); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics