Month: September 2021

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 61881-19-4 as follows. Application In Synthesis of 2,2,2-Trifluoro-N-phenylacetimidoyl chloride

4.3 3,4-Di-O-benzoyl-2-O-triisopropylsilyl-alpha-L-fucopyranosyl N-phenyltrifluoroacetimidate (6) To a solution of 3,4-di-O-benzoyl-2-O-triisopropylsilyl-L-fucopyranose (5) (0.25?g, 0.5?mmol) in CH2Cl2 (3.5?mL) CF3C(NPh)Cl [ 94 ] (0.37?mL, 2.2?mmol) and Cs2CO3 (290?mg, 0.9?mmol) were added at 0?C. The reaction mixture was stirred at 20?C for 20?h. Then the mixture was diluted with CHCl3 (50?mL), organic layer was separated and washed with H2O (50?mL), concentrated under reduced pressure and the residue dried in vacuo and purified by silica gel column chromatography (petroleum ether-EtOAc, 10:1???3:1) to give imidate 6 as a white foam (310?mg, 93%). [alpha]D23 -167.0 (c 1.0, CHCl3). Rf?=?0.71 (petroleum ether-EtOAc, 4:1). 1H NMR (300?MHz, CDCl3, delta, ppm, J, Hz): 0.73-1.10 (m, 21H, (CH3)2CH), 1.31 (d, 3H, J6,5 6.5, H-6), 4.50 (q, 1H, J5,6 6.5, H-5), 4.77 (dd, 1H, J2,1 3.5, J2,3 10.2, H-2), 5.70-5.85 (m, 2H, H-3, H-4), 6.58 (br.s, 1H, H-1), 6.80-6.95 (m, 2H, PhN (H-2, H-6)), 7.08-7.20 (m, 1H, PhN (H-4)), 7.24-7.40 (m, 4H, Ph), 7.46-7.57 (m, 3H, Ph), 7.59-7.70 (m, 1H, PhCO (H-4)), 7.78-7.87 (m, 2H, PhCO (H-2, H-6)), 8.04-8.15 (m, 2H, PhCO (H-2, H-6)). 13C NMR (75?MHz, CDCl3, delta, ppm, J, Hz): 12.4 ((CH3)2CH), 16.1 (C-6), 17.75, 17.78 ((CH3)2CH), 67.2 (C-2), 67.6 (C-5), 71.6, 71.7 (C-3 C-4), 95.4 (C-1), 116.2 (q, J 286.8, CF3), 119.4 (PhN (C-2, C-6)), 124.2 (PhN (C-4)), 128.1 (Ph (C-3, C-5)), 128.5 (Ph (C-3, C-5)), 128.7 (Ph (C-3, C-5)), 129.45 (PhCO (C-1)), 129.54 (PhCO (C-2, C-6)), 129.73 (PhCO (C-1)), 129.76 (PhCO (C-2, C-6)), 133.0, 133.4 (PhCO (C-4)), 143.6 (q, J 35.4, CF3C=N), 143.7 (PhN (C-1)), 165.67, 165.73 (CO). HRESIMS: found m/z 722.2729 [M+Na]+. Calcd for C37H44F3NNaO7Si: 722.2731. Found m/z 738.2468 [M+K]+. Calcd for C37H44F3KNO7Si: 738.2471.

According to the analysis of related databases, 61881-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Abronina, Polina I.; Zinin, Alexander I.; Romashin, Denis A.; Tereshina, Valeria V.; Chizhov, Alexander O.; Kononov, Leonid O.; Carbohydrate Research; vol. 464; (2018); p. 28 – 43;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 452-83-5,Some common heterocyclic compound, 452-83-5, name is 2-Chloro-5-fluoroaniline, molecular formula is C6H5ClFN, 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: NaOt-Bu (0.240 g, 2.5 mmol), Pd(OAc)2 (0.006 g, 0.025 mmol) and [HPt-Bu3][BF4] (0.010 g, 0.035 mmol) were suspended in toluene (3 ml) in a 5 ml microwave vial. The appropriate 2-chloroaniline (0.50 mmol) and aryl bromide (0.50 mmol) were then added and the vial sealed. The reaction was then heated in the microwave reactor at 160 C for 3 h, allowed to cool, and then quenched by addition of aqueous HCl (2 M, 3 ml). The organic phase was extracted with CH2Cl2 (2×20 ml), dried (MgSO4), then filtered and the solvent removed under reduced pressure. The crude product mixture was then subjected to column chromatography (SiO2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-5-fluoroaniline, its application will become more common.

Reference:
Article; Bedford, Robin B.; Bowen, John G.; Weeks, Amanda L.; Tetrahedron; vol. 69; 22; (2013); p. 4389 – 4394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 104-11-0, 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.

Example 111; N-(4-Chloro-benzyl)-2-(4-fluoro-phenyl)-N-methyl-4-[4-(2-oxo-pyrrolidin-1-yl)-piperidin-1-yl]-butyramide; a) Step 1; N-(4-Chloro-benzyl)-2-(4-fluoro-phenyl)-N-methyl-acetamide; A mixture of 1.09 g (7 mmol) 4-fluorophenylacetic acid, 1.37 g (9 mmol) (4-chloro-benzyl)-methyl-amine, 2.84 g (9 mmol) TBTU and 6 mL (35 mmol) DIPEA in 50 mL DMF was stirred at room temperature for 16 h. After evaporation of all volatiles Na2CO3 aq. was added and the mixture was extracted with ethyl acetate. The combined organic phases were washed with NaCl aq., dried with Na2SO4, filtered and evaporated to dryness. The residue was purified by column chromatography on silica eluting with a gradient formed from ethyl acetate and heptane. The product containing fractions were evaporated to yield 1.35 g (65%) of the title compound as yellow oil. MS(m/e): 292.2 (MH+).

The chemical industry reduces the impact on the environment during synthesis 1-(4-Chlorophenyl)-N-methylmethanamine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Knust, Henner; Nettekoven, Matthias; Ratni, Hasane; Vifian, Walter; Wu, Xihan; US2009/76081; (2009); 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 461-81-4 as follows. Computed Properties of C7H4ClF3O

a) Preparation of 4-trifluoromethoxybenzonitrile Process According to the Invention in MEK Under an atmosphere of nitrogen, a mixture of 6.5 g of bis-triphenylphosphine-nickel dichloride, 5 g of triphenylphosphine and 120 ml of MEK was stirred at room temperature for 10 minutes. 1.9 g of activated zinc powder were then added, and the reaction mixture was stirred at 70 C. for 30 minutes. Following this, the mixture was allowed to cool to 25 C., and 93.25 g of 1-chloro-4-trifluoromethoxybenzene were added dropwise. The mixture was stirred for 10 minutes, 24 g of sodium cyanide were added, and the reaction mixture was stirred at from 65 to 70 C. for 20 h. The conversion was then approximately 75% (GC). After cooling to room temperature, the mixture was filtered, the solid filter residue was washed 2* with 50 ml of MEK and the combined organic phases were concentrated under reduced pressure. Vacuum distillation gave 58.5 g (66% of theory) of 4-trifluoromethoxybenzonitrile as a colourless liquid (boiling point at 120 mbar: 80 C.). 2.6% of coupling products had formed.

According to the analysis of related databases, 461-81-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bayer Aktiengesellschaft; US6162942; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 870-24-6, These common heterocyclic compound, 870-24-6, name is 2-Chloroethanamine 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.

AEA was synthesised according to the method described by Jung et al. [22]. 2-chloroethylamine hydrochloride (5 g, 43 mmol) was ground and dissolved in deionised water (50 ml). Sodium azide (8 g, 123 mmol) was added and the mixture was heated at 80 C for 18 h. The solution was then made alkaline with potassium hydroxide (15 g), extracted using diethyl ether and dried over magnesium sulphate. Finally the solution was concentrated using rotary evaporation to give an amber coloured, viscous oil. AEA was characterised using 1H NMR and FTIR spectroscopy (See Fig. S1, Supporting information). The integrations for the peaks gave the correct proton ratios and the FTIR spectra (Fig. 2(a)) showed a strong azide band at 2100 cm-1.

Statistics shows that 2-Chloroethanamine hydrochloride is playing an increasingly important role. we look forward to future research findings about 870-24-6.

Reference:
Article; Farley, Robert; Saunders, Brian R.; Polymer; vol. 55; 2; (2014); p. 471 – 480;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

89794-02-5, name is 4-Bromo-2-chlorotoluene, 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: C7H6BrCl

General procedure: 10.0 mmol of the specified boronic ester (I; R1), 30.0 mmol of magnesium turnings and 10.0 mmol of the salt (II) were suspended in a mixture of 3.40 g of anhydrous toluene and 0.73 g of anhydrous tetrahydrofuran in a dry four-neck flask with a mechanical stirrer, thermometer, metal condenser and pressure-equalized dropping funnel under a nitrogen atmosphere, and stirred vigorously for 30 min. The appropriate haloaromatic (III, R4) was added to this solution, at first in undiluted form, until the onset of exothermicity signals the start of the reaction. The remaining total amount of 30.6 mmol of haloaromatic was diluted with 10.0 g of anhydrous toluene and 10.0 g of anhydrous tetrahydrofuran and added dropwise at such a rate that the internal temperature does not exceed 45 C. On completion of addition, the reaction mixture was heated at reflux for 1 h or until the dissolution of the magnesium was complete. The resulting suspension was discharged onto 50 g of ice-water, and the resulting solids are isolated, washed with cold water and dried under reduced pressure. Examples 15, 18, 20 and 27 and 46-52 were extracted from the aqueous phase with 100 ml of ethyl acetate, the solvent was distilled off under reduced pressure and the resulting oils were isolated. The isolated yield for Example 1 that was prepared by this method was 2.87 g (72% of theory), whereas Example 1 prepared according to DE 198 50 139 A1 was obtained in a yield of 47% of theory.The composition of Examples 1-76 and selected physical properties are summarized in Table 2.

The synthetic route of 89794-02-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Covestro Deutschland AG; ROeLLE, Thomas; BERNETH, Horst; HOeNEL, Dennis; BRUDER, Friedrich-Karl; (34 pag.)US2019/276479; (2019); 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. 1939-99-7, name is Phenylmethanesulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of Phenylmethanesulfonyl chloride

General procedure: Pyridine (73 lL, 0.90 mmol) and DMAP were added to a solution10a (203 mg, 0.7 mmol) in anhydrous DCM (10 mL). Then benzenesulfonylchloride (145 mg, 0.76 mmol) was dissolved in DCMand added dropwise under a nitrogen atmosphere. The reactionmixture was then stirred at room temperature for 1 day.Whereupon, HCl (1 mol/L) was added and the reaction mixturewas extracted with DCM. The organic phases were combined anddried over anhydrous Na2SO4. After removal of volatiles, a residuewas obtained that was then subjected to silica-gel column chromatographicpurification to afford this intermediate 13a (196 mg,63%).

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 1939-99-7.

Reference:
Article; Liu, Peihong; Du, Yongli; Song, Lianhua; Shen, Jingkang; Li, Qunyi; Bioorganic and Medicinal Chemistry; vol. 23; 21; (2015); p. 7079 – 7088;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 2453-46-5, 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. 2453-46-5, name is Chlorocycloheptane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 10 mL Schlenk tube was charged with CoBr2 (6.6 mg, 0.03mmol), 1,3-diisopropyl-1H-benzimidazol-3-ium bromide (L4; 8.5mg, 0.03 mmol), 4-methoxy-N-[(1E)-1-phenylethylidene]aniline(1a, 67.6 mg, 0.30 mmol), 1-chlorooctane (2a, 76.5 muL, 0.45 mmol), and THF (0.69 mL). A 1.92 M solution of t-BuCH2MgBr inTHF (0.31 mL, 0.60 mmol) was added dropwise at 0 C, and themixture was stirred at r.t. for 6 h. The reaction was quenched by theaddition of 3 M aq HCl (1.0 mL), and the mixture was stirred at r.t.for 1 h, then extracted with EtOAc (3 × 10 mL). The organic layerswere combined, dried (MgSO4), and concentrated under reduced pressure. The crude product was purified by chromatography [silicagel, hexane-EtOAc (40:1)].

The synthetic route of Chlorocycloheptane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Ke; Yamakawa, Takeshi; Yoshikai, Naohiko; Synthesis; vol. 46; 15; (2014); p. 2024 – 2039;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 1435-48-9,Some common heterocyclic compound, 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, molecular formula is C6H3Cl2F, 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.

448 mg of milled sodium hydroxide (1.4 eq; 0.0112 mmol), 1.32 g of 1,3-dichloro-4-fluorobenzene (1 eq; 0.008 mol) and 1.57 g of benzophenone hydrazone (1 eq; 0.008 mol) in 6 ml of degassed tert-amyl alcohol are loaded into a 20 ml reactor surmounted by a condenser, a mechanical stirrer and a temperature sensor, and placed in an inert atmosphere.8.95 mg of palladium acetate (0.001 mol %; 0.00004 mol) and 46.3 mg of 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (0.0008 mol) in 2 ml of degassed tert-amyl alcohol are loaded into a 100 ml Schlenk tube equipped with a magnetic stirrer and placed under an inert atmosphere.After stirring for twenty minutes, the catalyst thus prepared is transferred into the reactor.After stirring at 103 C. for 12 hours, the conversion of the 1,3-dichloro-4-fluorobenzene is complete and a benzophenone N-5-chloro-2-fluorophenylhydrazone yield of 85% (accompanied by 15% of benzophenone N-3-chloro-4-fluorophenylhydrazone) is measured by gas chromatography in the presence of an internal standard (hexacosane).

The synthetic route of 1435-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rhodia Chimie; US7557248; (2009); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 108-70-3, 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. 108-70-3, name is 1,3,5-Trichlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

n-Butyllithium (2.45 mL, 4.00 mmol) was added to a tetrahydrofuran (10 mL) solution of 1,3,5-trichlorobenzene(724 mg, 4.00 mmol) at -78C in an argon atmosphere, and the mixture was stirred for 45 minutes.[0146] After the addition of dimethylformamide (0.31 mL, 4.00 mmol) at -78C, the mixture was stirred for 45 minutes.[0147] After increasing the temperature of the mixture to -20C, a saturated ammonium chloride solution (5 mL) wasadded to the mixture, followed by stirring for 5 minutes.[0148] The organic layer was extracted with ethyl acetate, dried over sodium sulfate, and filtered, and the solvent wasevaporated.[0149] The residue was purified by silica gel column chromatography (15 g, hexane_acetone=50:1 to 40:1) to obtaina 2,4,6-trichlorobenzaldehyde compound (colorless crystals) (633 mg, 76%).Reference: Synthesis, 2008, 279-285.

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, 1,3,5-Trichlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; National University Corporation University Of Toyama; MORI Hisashi; TOYOOKA Naoki; MIZUGUCHI Mineyuki; OBITA Takayuki; HIRONO Syuichi; GODA Hiroaki; EP2808014; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics