Tag: M.W=100-200

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. 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 106131-61-7

To a solution of 3,6-dichloro-1,2,4,5-tetrazine (1.51 g, 10 mmol) in acetonitrile (70 ml) was added the sodium salt of 5-amino-1H-tetrazole (2.14 g, 10 mmol). The mixture was refluxed for 24 hours then allowed to cool to room temperature. The suspension was centrifuged until the supernatant liquid was clear. The liquid was decanted and the brown solid washed successively with acetonitrile and water. With each wash the solid was separated from the solvent by centrifugation followed by decantation. The isolated crude yield was 1.5 g (60%), this material was recrystallized from DMSO/methanol yielding an orange brown powder mp 264 C. dec; 1H NMR(deuteriomethylsulfoxide) 12.5(b,r s,4H); 13 C NMR (deuteriomethylsulfoxide) 151.74, 158.25; IR (KBr) 3421, 3000, 1615, 1436, 1127 cm-1. A gas pycnometer density of 1.76 g/cm3 was also determined and a drop height of 195 cm was measured (Type 12, HMX=24-27 cm).

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 106131-61-7.

Reference:
Patent; The Regents of the University of California; US6657059; (2003); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 932-96-7, 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. 932-96-7 name is 4-Chloro-N-methylaniline, 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.

General procedure: The reaction was carried out in a 10-mL stainless steel autoclave which was coupled with a magnetic stirrer. In a typical experiment for the N-formylation of amines with CO2 and hydrosilanes, N-methylaniline, the catalyst 3-PSZ-Br (or other catalysts when performing comparisons), and phenylsilane were added into the reactor. Subsequently, CO2 was charged into the reactor until the pressure reached 0.5 MPa and the reactor was then heated by an oil bath to 40 C while being stirred continuously. After the reaction, the autoclave was quickly cooled to 0 C and depressurized to atmospheric pressure [14]. The cycloaddition reactions with epoxides and CO2 were carried out in a similar fashion. Conversions and yields were determined using naphthalene or biphenyl as the internal standard and measured by a gas chromatograph (GC2010, Shimadzu Corporation, Japan) equipped with a capillary column (Rtx-5, 30 m ¡Á 0.32 mm ¡Á 0.25 mum) and a flame ionization detector (FID). The structure and the purity of the corresponding products were identified by 1H NMR, 13C NMR, and GC-MS analysis.

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

Reference:
Article; Zhang, Wuying; Luo, Rongchang; Xu, Qihang; Chen, Yaju; Lin, Xiaowei; Zhou, Xiantai; Ji, Hongbing; Cuihua Xuebao/Chinese Journal of Catalysis; vol. 38; 4; (2017); p. 736 – 744;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 57946-56-2, These common heterocyclic compound, 57946-56-2, name is 4-Chloro-2-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.

EXAMPLE 9 Production of the nitroaniline (XI): 4-Chloro-2-fluoroaniline (23 g) was dissolved in conc. sulfuric acid (120 ml), and the resultant mixture was cooled to -20 C., followed by dropwise addition of fuming nitric acid (15 g). The reaction mixture was stirred at -20 to -15 C. for 1.5 hours, poured into ice-water and then extracted with ether. The ether extract was washed with water and a saturated sodium bicarbonate solution, dried and concentrated. The residue was crystallized from a mixture of toluene and hexane (2:1) to obtain 20 g of 4-chloro-2-fluoro-5-nitroaniline. m.p., 83-84.5 C.

Statistics shows that 4-Chloro-2-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 57946-56-2.

Reference:
Patent; Sumitomo Chemical Company Limited; US4624699; (1986); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, 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 4090-55-5, Formula: C5H10ClO3P

Synthesis Example 3 (Synthesis of Phosphorus Compound 3); A mixture was obtained in the same manner as in Synthesis example 1 except that 114.4 g of toluene were used in place of 114.4 g of chlorobenzene, 161.5 g of 4-phenylphenol (para-phenylphenol) (0.95 mole) were used in place of 161.5 g of 2-phenylphenol (ortho-phenylphenol) (0.95 mole) and 127.5 g of toluene were used in place of 145.6 g of chlorobenzene to add to the reaction mixture.(After-treatment) The obtained mixture was cooled to room temperature and neutralized by adding a hydrochloric acid solution which corresponds to an excess amount of triethylamine, and allowed to stand to separate an oil phase. Next, the obtained oil phase was washed with approximately 85 C water and then any liquid was removed by a centrifugal filter. The obtained solid was dried by a vacuum desiccator at 100 C, to give 253.7 g of a white solid. The purity of the obtained solid was found to be 98.7 area % by GPC. Also, if all of the solids were assumed to be an object compound, the crude yield was 84.0 %. A structure of the obtained solid was determined according to results of quantitative analysis of phosphorus by elemental analysis and absorption spectrometry using an UV spectrometer, 1H-NMR, 13C-NMR and FT-IR, and the solid was identified as 5, 5-dimethyl-2-(4′-phenylphenoxy)-1, 3, 2-dioxaphosphorinane-2-oxide (phosphorus compound 3) of the below-mentioned constructional formula. Also, a melting point of the solid was measured in the same manner as in Synthesis example 1. Quantitative analysis of phosphorus by elemental analysis and absorption spectrometry (theoretical values in parentheses): Carbon: 64.3 % (64.2 %) Hydrogen: 6.1 % (6.0 %) Phosphorus: 9.7 % (9.7 %) Melting point: 165 to 167 CIR (KBr): 3008, 1606, 1523, 1488, 1405, 1376, 1296, 1226, 1194, 1174, 1114, 1059, 1002, 934, 861, 810, 765, 720, 691, 624 cm-1 3008, 1606, 1523, 1488, 1405, 1376, 1296, 1226, 1194, 1174, 1114, 1059, 1002, 934, 861, 810, 765, 720, 691, 624 cm-1 NMR: 1H-NMR (CDC13; 300MHz); delta 7.57-7.31 (9H, m, o-PP), 4.27 (2H, d, JHH=11Hz, POCH2C (CH3)2-), 4.01 (2H, dd, JHH=11Hz, JPH=22Hz, POCH2C (CH3)2-), 1.34 (3H, s, POCH2C (CH3)2-), 0.92 (3H, s, POCH2C (CH3)2-) ppm1H-NMR (CDC13; 300MHz); delta 7.57-7.31 (9H, m, o-PP), 4.27 (2H, d, JHH=11Hz, POCH2C (CH3)2-), 4.01 (2H, dd, JHH=11Hz, JPH=22Hz, POCH2C (CH3)2-), 1.34 (3H, s, POCH2C (CH3)2-), 0.92 (3H, s, POCH2C (CH3)2-) ppm13C-NMR (CDC13; 75MHz); delta 149.7 (d, 2JPC=6Hz), 140.0, 138.1, 128.7, 128.4, 127.2, 126.9, 119.7 (d, 3JPC=5Hz) (o-PP), 78.3 (d, 2JPC=7Hz, POCH2C (CH3)2-), 32.1 (d, 2JPC=6Hz, POCH2C (CH3)2-), 21.6, 20.1 ppm

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, 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1925622; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 104-11-0, These common heterocyclic compound, 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, 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.

Example 46: To a solution of Example 45 (30 mg, 75.9 umol, 1 eq) in CH3CN (1 mL) was added TMSC1 (24.7 mg, 227.6 umol, 28.8 uL, 3 eq) and Nal (34.1 mg, 227.6 umol, 3 eq) successively. The mixture was stirred at 25 C for 15 min. l-(4-chlorophenyl)-N-methyl- methanamine (18.9 mg, 121.4 umol, 1.20 eq) was then added and stirring continued for a further 10 min. NaBH(OAc)3 (64.3 mg, 303.5 umol, 3 eq) was added and stirring continued for 2 hours. The residue was diluted with water (10 mL) and extracted with EtOAc (5 mL *3). The combined organic layers were dried and the solvent removed in vacuo to afford the crude product. The crude product was purified by Prep-TLC on silica gel to give the target compound as a yellow solid (30 mg, 58.5%). LCMS MH+ calculated, 507.2, found, 507.2. 1H MR (400MHz, CD3OD) delta 8.81 – 8.71 (m, 1H), 8.19 (br s, 1H), 7.86 (br d, J=4.4 Hz, 1H), 7.54 – 7.46 (m, 8H), 7.39 (d, J=8.4 Hz, 2H), 4.75 (br t, J=6.8 Hz, 2H), 4.21 (s, 4H), 4.06 (s, 2H), 4.00 – 3.93 (m, 3H), 3.21 – 3.12 (m, 2H), 3.05 – 2.92 (m, 4H).

The synthetic route of 104-11-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHRYSALIS, INC.; GWALTNEY, Stephen; (167 pag.)WO2017/143011; (2017); 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. 13078-79-0, name is 2-(3-Chlorophenyl)ethanamine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 13078-79-0

Example 4; [0215] 14-[2-(3-Chlorophenyl)ethylearbamoyllthiazol-2-ylmethyllcarbamic acid tert- butyl ester: 2- (Boc-aminomethyl)thiazole-4-carboxylic (0.5 g, 1.9 mmol) and HATU (0.81 g, 2.1 mmol) were weighed into a flask. DMF (7 mL) and DIEA (0.68 mL, 3.9 mmol) were added. The mixture was stirred for 10 minutes. 2-(3- Chlorophenyl)ethylamine (0.3 g, 1.9 mmol) was added and reaction mixture was stirred for 12 hours. The mixture was diluted EtOAc and water. The layers were separated and the aquous layer was extracted with 3 x EtOAc. The combined organic layers were washed with 5% aqueous lithium chloride and brine, dried over sodium sulfate, filtered, and concntrated in vacuo. The material was purifed by filtration through a plug of silica gel with 1: 1 EtOAc: hexane to afford the title compound (0.73 g, 95%) : 1H NMR (400 MHz, d6-DMSO) : 8.42 (t, 1H), 8.10 (s, 1H), 7.85 (t, 1H), 7.27 (m, 3H), 7.16 (m, 1H), 4.38 (d, 2H), 3.46 (q, 2H), 2.82 (t, 2H), 1.39 (s, 9H) ; MS (ESI-LCMS) for C14H14ClN3O3S: 340 (MH-tBu+).

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 13078-79-0.

Reference:
Patent; EXELIXIS, INC.; WO2005/97765; (2005); 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. 98446-49-2, name is 2,4-Dichloro-5-methoxyaniline, A new synthetic method of this compound is introduced below., Computed Properties of C7H7Cl2NO

EXAMPLE 4 Preparation of 4-[(2,4-dichloro-5-methoxyphenyl)amino]-5-(3,4-dimethoxyphenyl)nicotinonitrile 137 A mixture of 4-chloro-5-(3,4-dimethoxyphenyl)nicotinonitrile (0.5 g, 1.82 mmol), 2,4-dichloro-5-methoxyaniline (0.402 g, 2.1 mmol), Pd2(dba)3 (0.167 g, 0.18 mmol), 2-dicyclohexylphosino-2′-(N,N-dimethylamino)biphenyl (0.22 g, 0.56 mmol), and K3PO4 (0.58 g, 2.73 mmol) in 10 ml of DME was heated at reflux for 45 minutes. The hot mixture was filtered and solids were washed with ether. The combined filtrates were washed with saturated NaHCO3, dried (MgSO4), and filtered through a pad of Magnesol. Solvent was removed and the residue was chromatographed on silica gel. Product was eluted with CH2Cl2-ether and then recrystallized from iso-propanol/hexane giving 0.21 g of 4-[(2,4-dichloro-5-methoxyphenyl)amino]-5-(3,4-dimethoxyphenyl)nicotinonitrile 137. HPLC retention time(a): 0.86 min.; MS: 430.2 m/e (M+H). Following procedures analogous to those described for the preparation of compound 137 and using the appropriate aniline, the compounds in Table 3 were prepared.

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; Cole, Derek Cecil; Asselin, Magda; Boschelli, Diane Harris; Wissner, Allan; Wang, Yanong Daniel; Prashad, Amarnauth Shastrie; Dushin, Russell; US2007/287738; (2007); 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. 2687-12-9, name is Cinnamyl chloride, A new synthetic method of this compound is introduced below., Safety of Cinnamyl chloride

To a solution of 2.94 g (0.02 mol) of isatin in 20 mL of DMF with stirring at 10C was slowly added 0.84 g (0.02 mol) of sodium hydride (60% suspension in mineral oil). After 30 min, 2.92 mL (0.02 mol) of cinnamyl chloride was added to the resulting purple solution followed by stirring at room temperature for 3 h. The reaction mixture was poured into 100 g of crushed ice. Next, the resulting precipitate was filtered off, washed with hexane, and dried in a vacuum(18 mmHg).

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

Reference:
Article; Bogdanov; Sadykov; Musin; Khamatgalimov; Krivolapov; Dobrynin; Mironov; Russian Journal of General Chemistry; vol. 85; 9; (2015); p. 2030 – 2036; Zh. Obshch. Khim.; vol. 85; 9; (2015); p. 1446 – 1452,7;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 13726-14-2, name is 4-Chloro-3-methoxyaniline, 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 13726-14-2, Recommanded Product: 13726-14-2

A mixture of ethyl 2,4-dichloropyrimidine-5-carboxylate (0.442 g, 2.0 mmol), 4-chloro-3- methoxyaniline (0.331 g, 2.1 mmol), DIPEA (0.42 mL, 2.4 mmol), and iPrOH (2 mL) was added to a 5 mL microwave vial which was then sealed and placed in a hot oil bath with stirring at 85 C overnight for 17 hours. At this point, a brown solid had formed and this was then washed with iPrOH (10 mL), water (10 mL), iPrOH (10 mL), and hexanes (10 mL) to yield RJ1-061 as a brown solid (0.570 g, 83%). m.p. = 119 C (decomposed). NMR (400 MHz, DMSO-ifc) delta 10.27 (s, 1H), 8.81 (s, 1H), 7.48 (d, / = 2.3 Hz, 1H), 7.43 (d, / = 8.6 Hz, 1H), 7.28 (dd, / = 8.6, 2.3 Hz, 1H), 4.37 (q, / = 7.1 Hz, 2H), 3.85 (s, 3H), 1.34 (t, / = 7.1 Hz, 3H). LRMS (ESI+) m/z 342.1 (MC135C135+H)+, 344.0 (MC135C137+H)+, 346.0 (MC137C137+H)+; (ESI-) m/z 339.3 (MC135C135-H)-; HRMS (ESI+) m/z calculated for C14H13CI2N3O3 (M+H)+ 342.04067, found 342.04100.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; H. LEE MOFFITT CANCER CENTER & RESEARCH INSTITUTE, INC.; SCHOeNBRUNN, Ernst; LAWRENCE, Nicholas J.; LAWRENCE, Harshani R.; (293 pag.)WO2017/66428; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 367-22-6, name is 4-Chloro-3-fluoroaniline, 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 367-22-6, Computed Properties of C6H5ClFN

To 4-chloro-3-fluoroaniline (25g, 0.17 mmol) in 250 mL of H2O was added NaHCO3 (21.6g, 0.25 mmol). After cooling to 0 C, iodine (43.5 g, 0.17 mmol) was added. After 18 h at rt, an additional 10.8 g of iodine was added and the reaction was stirred overnight. The reaction was extracted with DCM (4×250 mL), the combined organics were washed with sodium thiosulfate solution (2×250 mL) and brine (2×250 mL) and dried (Na2SO4). Purification by silica gel chromatography gave 47 g of Intermediate 5A. MS (ESI) m/z: 145.2 (M+H)+.

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-Chloro-3-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ORWAT, Michael J.; PINTO, Donald J.P.; SMITH II, Leon M.; SRIVASTAVA, Shefali; WO2013/56060; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics