Tag: M.W=100-200

Synthetic Route of 7051-16-3, A common heterocyclic compound, 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene, molecular formula is C8H9ClO2, 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.

1.0 M solution of boron tribromide in DCM (12.00 mL, 11.49 mmol) was slowly added to a solution of 5-chloro-1,3-dimethoxybenzene 28 (1.00 g, 5.74 mmol) in DCM (10.00 mL) at -78 C. After reaction was allowed to gradually warm to room temperature, the mixture was stirred for 2 days until no starting material was observed by TLC. Reaction mixture was diluted with NaHCO3 (aq. sat.) (50.00 mL) and reaction product was extracted with DCM (3 x 50.00 mL). The combined organic extract was washed with NaCl(sat. aq.) (20.00 mL), dried over anhydrous Na2SO4, and filtered. Obtained supernatant was concentrated under reduced pressure and crude residue was purified by flash column chromatography using n-hexane/ethyl acetate (7:3) to give 5-chlororesorcinol 28b (0.80 g, 96%) as a brown residue. 1H NMR (400 MHz, CDCl3-d) deltaH 6.21 (s, 1H, ArH), 6.37 (d, 2H, J = 2.2 Hz, ArH).

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:
Article; Hossain, Mohammad Anwar; Sattenapally, Narsimha; Parikh, Hardik I.; Li, Wei; Rumbaugh, Kendra P.; German, Nadezhda A.; European Journal of Medicinal Chemistry; vol. 185; (2020);,
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Related Products of 821-10-3, 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. 821-10-3, name is 1,4-Dichlorobut-2-yne belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: K2CO3 (3a, 210 mg, 1.5 mmol) was added to a solution of b-ketosulfones 1a-p (0.5 mmol) in acetone (10 mL) at 25 C. The reaction mixture was stirred at 25 C for 10 min. 1,4-Dichloro-2-butyne (2, 68 mg, 0.55 mmol) was added to the reaction mixture at 25 C. The reaction mixture was stirred at 56 C for 8 h. The reaction mixture was cooled to 25 C and the solvent was concentrated. The residue was diluted with water (10 mL) and the mixture was extracted with CH2Cl2 (320 mL). The combined organic layers were washed with brine, dried, filtered and evaporated to afford crude product. Purification on silica gel (hexanes/EtOAc15/1e8/1) afforded 4a-p.

The synthetic route of 1,4-Dichlorobut-2-yne has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chan, Chieh-Kai; Lu, Yi-Ju; Chang, Meng-Yang; Tetrahedron; vol. 71; 51; (2015); p. 9544 – 9549;,
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These common heterocyclic compound, 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, 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: C10H13Cl

The method for synthesizing the aphid butyl fluoride ester intermediate p-tert-butyl phenylacetonitrile comprises the following steps: 1) Under argon conditions,Ethyl acetonitrile,Potassium tert-butoxide,Mix the t-butanol,Warming up to 98 ¡ã C,The control pressure is 4.5 atmospheres.Within 30min1 mol of tert-butylchlorobenzene and DMSO solution were added in 3 batches,Then control the reaction temperature to 112 ¡ã C,The reaction pressure is 5 atmospheres.The reaction ended at 2.5h.Then add deionized water,Control reaction temperature is 142¡ãC, the reaction pressure is 8 atmospheres,Continue the reaction 5h end;The ratio of 4-tert-butylchlorobenzene to ethyl cyanoacetate is 1:1.35,The amount of ethyl cyanoacetate and potassium t-butoxide is 1:1.55,The ratio of ethyl cyanoacetate to tert-butanol is 1g: 10ml,The ratio of 4-tert-butylchlorobenzene to DMSO is 1g: 5ml.The ratio of potassium t-butoxide to deionized water is 1:11.2) The system removes the solvent by a rotary evaporator.Then transfer the residue to the water,Add toluene and stir,The layers were separated, and the organic phase was collected and dried over anhydrous sodium sulfate.Then the filtrate was collected by filtration.The filtrate was distilled under reduced pressure to collect a fraction of 78 to 79 ¡ã C (0.1 torr).The product was obtained in a molar yield of 97.7percent and an HPLC purity of 98.9percent.

The synthetic route of 1-tert-Butyl-4-chlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shandong Nong Pharmaceutical Xue Institute; Jinan Kehai Co., Ltd.; Yang Chaohui; Fu Hongxin; Wang Ling; (6 pag.)CN109053491; (2018); A;,
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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. 39989-43-0, name is 3,5-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., Application In Synthesis of 3,5-Dichlorobenzylamine

iV-(3,5-Dichlorobenzyl)-5-fluoro-2-(methylsulfonyl)benzenamine:; A mixture of 2,4-difluoromethylsulfonylbenzene (5.0 mmol), 3,5-dichlorobenzylaniine (5.0 mmol), LambdazetaiV-diisopropylethylamine (10.0 mmol) and acetonitrile (25 mL) was heated at reflux for 18 h, cooled and concentrated in vacuo. The residue was dissolved in ethyl acetate; this solution was washed with water, dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using 5 % ethyl acetate in hexanes as eluent to yield the title compounds as a yellowish solid (37 %). 1H NMR (400 MHz, CDCl3): delta 9.28 (br s, 1 H), 7.88 (m, 1 H), 7.34 (s, 1 H), 7.22 (s, 2 H)5 6.44 (m, 1 H)3 6.30 (dd, 1 H), 4.43 (d, 2 H).

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; PREDIX PHARMACEUTICALS HOLDINGS, INC.; WO2006/81332; (2006); A1;,
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Electric Literature of 363-51-9, 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. 363-51-9, name is 2-Chloro-6-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of triphosgene (408 mg, 1.37 mmol) in DCM (3 ml) was added 2-chloro-6-fluoro-aniline (200 mg, 1.37 mmol). The RM was cooled to 0 C and treated with triethylamine (402 mu, 2.89 mmol). The RM was stirred at rt for 1 h. The solvent was removed under reduced pressure to give the desired product as a white solid and it was used in the next step without further purification. MS ES+: 204.2 (in methanol).

The synthetic route of 2-Chloro-6-fluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NODTHERA LIMITED; BOCK, Mark G.; WATT, Alan Paul; PORTER, Roderick Alan; HARRISON, David; (229 pag.)WO2019/25467; (2019); A1;,
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Application of 4584-46-7, These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine 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.

In a 250 mL three-necked flask, 20 g of 2-dimethylaminochloroethane hydrochloride (139 mmol) was added,150 mL of DMF-H2O mixed solution (v/v: 7:3),10 grams of sodium azide (154 mmol) and a catalytic amount of NaI.The reaction solution was heated to 80 C., incubated for 36 h, and cooled to room temperature.The reaction solution was neutralized with sodium carbonate, and then the pH of the reaction solution was adjusted to 11 with sodium hydroxide.Add 100 mL of ethyl acetate and extract three times with 180 mL of ethyl ether to combine the organic phase.Dry over anhydrous magnesium sulfate, filter, and evaporate the solvent ether under reduced pressure at room temperature.Add 100g to the above residual ethyl acetate solution1-Iodine-1H,1H,2H,2H-perfluorodecane (174 mmol), warmed to 75C, and reacted overnight to precipitate a yellow solid, the supernatant was removed, and the solid was washed three times with ethyl acetate in a vacuum. After drying for 2 days, a fluoromonomer modified by a click functional group was obtained.

The synthetic route of 4584-46-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Keerbo New Materials Technology Co., Ltd.; Hu Jianqing; Peng Kaimei; Deng Jian; Guo Hongwei; (17 pag.)CN107573250; (2018); A;,
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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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, A new synthetic method of this compound is introduced below., Quality Control of 3-Chloro-2-chloromethyl-1-propene

Sodium hydride (60% in mineral oil) (0.99 g, 24.81 mmol) was dissolved in DMF (20 mL) at 0 C and 3-chloro-2-(chloromethyl)prop-1-ene (1.31 mL, 12.41 mmol) was added in portions. Separately N-boc-ethanolamine (1.92 mL, 12.41 mmol) was dissolved in THF (20 mL) and added dropwise. The reaction mixture was stirried at 20 C for 21 h. The volatiles were removed under reduced pressure. The reaction was diluted with water (50 mL) and then extracted with EtOAc (3 x 80 mL). The organic extracts were combined passed through a phase separation cartridge and the volatiles were removed under reduced pressure. The crude product was dissolved in DCM and purified via silica gel chromatography eluting with 0-50% EtOAc in heptane to afford tert-butyl 6-methylene-1,4-oxazepane-4-carboxylate (1.25 g, 47%) as a clear oil. 1H NMR (400 MHz, CDCl3) 1.46 (s, 9H), 3.37 – 3.45 (m, 2H), 3.64 – 3.79 (m, 2H), 4.00 – 4.24 (m, 4H), 4.88 – 5.04 (m, 2H); 13C NMR (400 MHz, DMSO, 100 C) 28.58, 50.40, 51.72, 71.82, 74.29, 79.44, 112.06, 146.96, 154.80; HRMS [M+H]+ measured 236.1274, C11H19NO3 requires 236.1263.

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:
Article; Watson, David W.; Gill, Matthew; Kemmitt, Paul; Lamont, Scott G.; Popescu, Mihai V.; Simpson, Iain; Tetrahedron Letters; vol. 59; 51; (2018); p. 4479 – 4482;,
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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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-(Chloromethyl)benzo[d][1,3]dioxole

To a slurry of magnesium turnings (1.09 g, 44.8 mmol) in 5 mL of THF was added iodine (0.0650 g, 0.256 mmol), followed by a solution of 5-(chloromethyl)benzo[d][l,3]dioxole. (6.55 g, 38.4 mmol) in 30 mL of THF. After 1 minute, the exothermic reaction mixture was placed in an ice bath for 1 minute and then stirred at ambient temperature for 1 hour. TMEDA (7.68 ml, 51.2 mmol) was added to the reaction and the mixture was cooled to -78 0C for 5 minutes at which point a solution of (E)-N-((S)-2,3-bis(tert- butyldimethylsilyloxy)propylidene)-2-methylpropane-2-sulfinamide (5400 mg, 12.8 mmol) in 25 mL THF was added via a syring pump over 15 minutes. The reaction was allowed to warm to RT over the course of 2 hours then stirerd at RT for an additional hour. The mixture was diluted with ethyl acetate (10O mL) and poured in saturated ammonium chloride (250 mL). The aqueous layer was extracted with ethyl acetate (2 x 250 mL) and the combined organic layers were washed with water and then brine and dried over Na2Stheta4. The organic colvents were filtered, concentrated under reduced pressure and the crude material was purified by silica gel to provide N-((2R,3 S)-I- (benzo[d][l,3]dioxol-5-yl)-3,4-bis(tert-butyldimethylsilyloxy)butan-2-yl)-2- methylpropane-2-sulfinamide (4.51 g, 63.1% yield) as a colorless oil.

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AMGEN INC.; WO2008/147547; (2008); A1;,
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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. 95-49-8, name is 1-Chloro-2-methylbenzene, A new synthetic method of this compound is introduced below., name: 1-Chloro-2-methylbenzene

In a 250 mL four-necked flask was added 141 mL (150 g) o-chlorotoluene, adding 3.0 g Hbeta molecular sieve catalyst, stirring to disperse evenly; and then into the system by 50 mL / min sulfuric acid dry chlorine gas, at 35 C for 12 h to give dichlorotoluene. After the exhaust gas is condensed, the unreacted Cl2 is removed by the NaOH solution.

The synthetic route of 95-49-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing Zhongteng Chemical Co., Ltd.; Zhong Hua; Lu Minshan; Chen Xiuzhen; Liu Qiaobao; Yin Hengbo; Wang Aili; (8 pag.)CN104876790; (2017); B;,
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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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 14752-66-0

(b) Sodium 4-chlorophenylsulfi nate [9.93 g(0.05 mol)] and monochloroacetic acid [4.72 g(0.05 mol)] were dissolved in 20 mL of water, adjustedto pH 10 with a NaOH solution, and boiled in a waterbath for 1 h. The reaction mixture was cooled, and extractedwith benzene (2 ¡Á 30 mL). From the benzenesolution, after distilling off the solvent, 0.67 g (7%)of sulfone (3), i.e., 4-lC6H4SO2CH3 was obtained,mp 93-95C. Found, %: 44.30, 3.58, Cl 18.41,S 16.67. 77Cl2S. Calculated (%): 44.10, 3.71,Cl 18.59, S 16.82The aqueous layer was acidifi ed with HCl untilneutral and held at 5C for 12 h. The precipitate wasrecrystallized (chloroform-hexane, 1 : 2) and dried invacuo over P2O5. 10.78 g (92%) of acid (1) was obtained,mp 120-122C.

According to the analysis of related databases, 14752-66-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Adamovich; Oborina; Mirskova; Russian Journal of Applied Chemistry; vol. 91; 4; (2018); p. 701 – 705; Zh. Prikl. Khim. (S.-Peterburg, Russ. Fed.); vol. 91; (2018); p. 602 – 606,5;,
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