Tag: M.W=200-300

Related Products of 108649-59-8,Some common heterocyclic compound, 108649-59-8, name is 1-(2-Bromoethyl)-2,4-dichlorobenzene, molecular formula is C8H7BrCl2, 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.

Step i: Synthesis of 2-bromo-5-(2,4-dichlorophenethyl)-4,5,6 ,7-tetrahvdrothiazolo[5,4-clpyridine A mixture of l-(2-bromoethyl)-2,4-dichlorobenzene (0.1 g, 0.000393 mol) and 2-bromo-4,5,6,7- tetrahydrothiazolo[5,4-c]pyridine(0.103 g, 0.000472 mol) in DMF (2 mL) was cooled to 0 – 5 C, and added NaH (0.014 g, 0.00059 mol). The RM was then warmed to 60 C for 6 h. The RM was cooled to RT, quenched with water, extracted into ethyl acetate and organic portion was washed with water, dried over sodium sulphate, concentrated to get the titled compound (0.06g, 38.2%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(2-Bromoethyl)-2,4-dichlorobenzene, its application will become more common.

Reference:
Patent; AURIGENE DISCOVERY TECHNOLOGIES LIMITED; KOTRABASAIAH UJJINAMATADA, Ravi; HOSAHALLI, Subramanya; BEJUGAM, Mallesham; WO2015/101928; (2015); A1;,
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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. 873-38-1, name is 2-Bromo-4-chloroaniline, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Bromo-4-chloroaniline

2-Bromo-4-chloroaniline (1.0 eq) was dissolved in CH2Cl2(0.25M), then triethylamine and triflouroacetyl anhydride (1.1 eq each) were added. The resulting mixture was stirred at room temperature for 1 hour. Solvent was then stripped-off from the reaction mixture, and the residue was purified by flash chromatography with dichloromethane as eluent to give the described product in 97% yield. m/z(M-H) -300.0.

According to the analysis of related databases, 873-38-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wyeth; US2008/9485; (2008); A1;,
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Synthetic Route of 13745-86-3, These common heterocyclic compound, 13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine, 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 1 Preparation of 1 l-piperazin-l-yldibenzor&,/iri,4~lthiazepineInto a 1000 mL round-bottom flask equipped with a magnetic stirring bar and reflux condenser with a nitrogen inlet was charged with 25.0 grams (g) (0.110 mole) of dibenzo[b,fj[l,4]thiazepine-l l(10-H)-one (made by the method disclosed by J. Schmutz et al. HeIv. Chim. Acta., 48: 336 (1965)), as a dry solid, followed by 310 mL POCl3 and 3 mL of N,N-dimethylaniline. The reaction mixture was heated at reflux (106 degrees C) for 6 hours giving a clear orange solution. The reaction was then cooled to room temperature, and POCl3 removed on the rotary evaporator leaving an orange oil. This residue was partitioned between ice -water (500 mL) and ethyl acetate (800 mL). The layers were separated and the aqueous phase extracted with ethyl acetate (3 X 200 mL). The combined ethyl acetate extracts were dried over MgSO4 , filtered, and then stripped down on the rotary evaporator, leaving the crude imino chloride as a light yellow solid (26.26g, 97% yield). The structure was confirmed by NMR and Mass Spectrum (300 MHz, CDCl3; ES+, M+l = 246.7). Crude imino chloride (27.35 g, 0.111 mole) was added to 1000 mL o-xylene in a 2000 mL round-bottom flask equipped with a magnetic stir bar and a reflux condenser with nitrogen inlet. To this solution was added commercially available piperazine (47.95g, 0.557 mole) in one portion as a dry solid at room temperature. The mixture was stirred until nearly all the piperazine dissolved. EPO Then the reaction mixture was heated at reflux (142 degrees C) for 40 hours (out of convenience). The reaction was then allowed to cool to room temperature, and an aliquot was partitioned between IN NaOH / CH2Cl2. The organic phase was checked by TLC (silica gel, CH2Cl2 / Methanol 90:10, iodoplatinate visualized) and showed clean conversion to one major product (Rf = 0.45). A drop of the reaction solution was diluted with CH3CN to prepare a sample for LC / MS analysis, which confirmed the presence of the desired product (M+l = 296.4). The reaction mixture was stripped down on the rotary evaporator under high vacuum to remove the xylene. The residue was partitioned between IN NaOH (400 mL) and CH2Cl2 (200 mL). The layers were separated, and the aqueous phase further extracted with CH2Cl2 (3 X 200 mL). The combined CH2Cl2 extracts were washed with brine (200 mL), then dried over MgSO4, filtered, and stripped down on the rotary evaporator to give the crude title compound as a yellow gum (35.3 g). The crude free base was purified by flash column chromatography over silica gel (600 g) eluting with a gradient of 0 to 20% Methanol in CH2Cl2. Fractions containing the pure desired product were combined and stripped down on the rotary evaporator, to afford the purified free base as a light yellow foam (25.67g, 78% yield).

The synthetic route of 13745-86-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2006/73360; (2006); A1;,
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Reference of 928783-85-1,Some common heterocyclic compound, 928783-85-1, name is 1-Bromo-3-chloro-5-(trifluoromethyl)benzene, molecular formula is C7H3BrClF3, 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 500 ml multineck flask with low-temperature thermometer, dropping funnel and argon balloon, 5.5 g (0.228 mol, 1.3 eq) of magnesium turnings (activated with dibromoethane and washed with diethyl ether) were blanketed with 120 ml of diethyl ether. At 0 C., 45.5 g of 3-bromo-5-chlorobenzotrifluoride (0.175 mol, 1 eq) in 120 ml of diethyl ether were slowly added dropwise. The reaction started up of its own accord after a few minutes, with a colour change (red-brown) and heating; the temperature was kept at about 0 C. during the addition. On completion of addition of the bromide, the mixture was stirred for a further 30 min.A separate 2 l 3-neck flask with low-temperature thermometer, dropping funnel and argon balloon was initially charged with 32.4 g of ethyl trifluoroacetate (0.228 mol, 1.3 eq) in 250 ml of diethyl ether, and cooled to -80 C. At this temperature, the Grignard reagent (cooled to -10 C.) was slowly added dropwise. On completion of addition, the reaction mixture was stirred at -80 C. for a further 30 min. Thereafter, the reaction mixture was warmed to -10 C. and acidified with 10% hydrochloric acid. The resulting mixture was admixed with saturated NaCl solution, the phases were separated and the aqueous phase was washed with 200-300 ml of diethyl ether. The combined ethereal phases were dried over magnesium sulphate and the solvent was subsequently removed on a rotary evaporator.The resulting crude product was purified by vacuum distillation (71 C. at 18 mbar). 37.7 g (78% of theory) of 1-[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroethanone were obtained as a colourless oil. This was converted further without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3-chloro-5-(trifluoromethyl)benzene, its application will become more common.

Reference:
Patent; Bayer CropScience AG; US2011/105532; (2011); A1;,
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Related Products of 61881-19-4, 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. 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, This compound has unique chemical properties. The synthetic route is as follows.

Cs2C03 (3.0 equiv.), CF3C(NPh)CI (3.0 equiv.) were added to a stirred solution of 22 in DCM (10 mL/1 g) at 0C. After 10 min., the mixture was brought to rt and stirred for 1 h. After complete consumption of 22, reaction mixture was filtered, and the filtrate was concentrated. The obtained crude residue was purified by automated flash column chromatography on silica gel (0-60% EtOAc in cyclohexane) to afford the desired imidate donor 23 (87%) as foam.

The chemical industry reduces the impact on the environment during synthesis 2,2,2-Trifluoro-N-phenylacetimidoyl chloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; VAXXILON AG; EMMADI, Madhu; LISBOA, Marilda P; KNOPP, Daniel; MONNANDA, Bopanna; VON BONIN, Arne; PEREIRA, Claney Lebev; (309 pag.)WO2020/104697; (2020); A1;,
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Reference of 172921-33-4,Some common heterocyclic compound, 172921-33-4, name is 1-Bromo-4-chloro-2,5-difluorobenzene, molecular formula is C6H2BrClF2, 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.

To a solution of 1-bromo-4-chloro-2,5-difluorobenzene (200 mg, 0.879 mmol) in THF (10 mL) cooled to -10¡ãC was added isopropylmagnesium bromide (1M in THF, 1.055 mL, 1.055 mmol) dropwise and the reaction mixture was stirred at this temperature for 1 h. The reaction mixture was then warmed to 0 ¡ãC and stirred for another 1 h. The resultant mixture was again cooled to -10 ¡ãC and treated dropwise with a solution of 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (196 mg, 1.055 mmol). The reaction mixture was allowed to warm up to room temperature and treated with a saturated solution of ammonium chloride (3 mL). The layers were separated and aqueous layer was extracted with dichloromethane (2×2 mL). The combined organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to afford crude compound which was purified by column chromatography on a silica (7:3 – Ethyl acetate:hexane) to afford 2-(4-chloro-2,5-difluorophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (150 mg, 0.546 mmol, 62percent yield) as an oil.

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

Reference:
Patent; Bristol – Myers Squibb Company; Vivekanand, M.Burda; Pan, Senrian; Ramkumar, Rajamani; Sushil, Jetanand Nara; Maheswaran, Shibasanban Calatrava; Tarun Kumar, Meishar; Jonathan, L. Ditta; Carolyn, Diane Jiaba; John, J. Bronson; John, E. Maco; (232 pag.)JP2015/528018; (2015); A;,
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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. 328-84-7, name is 3,4-Dichlorobenzotrifluoride, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3,4-Dichlorobenzotrifluoride

PRODUCTION EXAMPLE 3 Production of an Intermediate Aniline Compound 5.00 Grams of 5-chloro-2-fluoro-4-mercaptoaniline, 12.2 g of 3,4-dichlorobenzotrifluoride and 4.31 g of potassium carbonate were dissolved in 30 ml of dimethylformamide, and the resulting solution was stirred for 2 hours at a temperature of from 100 to 110 C. in an oil bath. Thereafter, the reaction solution was poured into water and extracted with three 200-ml portions of diethyl ether. The extract obtained was washed with water, dried, filtered and concentrated. The residue obtained was subjected to chromatography on silica gel to obtain 6.57 g of 5-chloro-2-fluoro-4-[2-chloro-4-(trifluoromethyl)phenylthio]aniline. Yield 66% m.p. 80.8 C. 1 H-NMR (CDCl3):

According to the analysis of related databases, 328-84-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sumitomo Chemical Company, Limited; US5116875; (1992); 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. 220227-21-4, name is 2,4,5-Trifluorobenzene-1-sulfonyl chloride, A new synthetic method of this compound is introduced below., SDS of cas: 220227-21-4

General procedure: To a solution of A/-(2,4-dimethoxybenzyl)-3-methyl-1 ,2,4-thiadiazol-5- amine (1.14 g, 4.30 mmol) in tetrahydrofuran (20 mL) was added lithium N’s(trimethylsilyl)amide (1 M solution in tetrahydrofuran, 4.3 mL, 4.3 mmol) at -78 C. The reaction mixture was stirred for 30 minutes at 0 C and a solution of 2,4,5- trifluorobenzenesulfonyl chloride (0.99 g, 4.30 mmol) in tetrahydrofuran (10 mL) was added dropwise at -78 C. After the addition was complete, the cooling bath was removed. The reaction mixture was stirred for 3 h at ambient temperature and saturated aqueous ammonium chloride (10 mL) was added. The mixture was extracted with ethyl acetate (2 x 30 mL). The organic layer was washed with water and brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo and the residue was purified by column chromatography eluting with 30% ethyl acetate in hexanes to afford A/-(2,4-dimethoxybenzyl)-2,4,5-trifluoro-A/-(3-methyl- 1 ,2,4-thiadiazol-5-y)benzenesulfonamide in 42% yield (0.83 g) as a colorless solid: MS (ES+) m/z 459.8 (M + 1).

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; XENON PHARMACEUTICALS INC.; SUN, Shaoyi; ZENOVA, Alla, Yurevna; CHAFEEV, Mikhail; JIA, Qi; ZHANG, Zaihui; OBALLA, Renata, Marcella; WO2013/64983; (2013); A1;,
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These common heterocyclic compound, 928782-97-2, name is 4-Chloro-2-(phenylethynyl)aniline, 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. Product Details of 928782-97-2

General procedure: Therequisite 2-alkynylaniline derivatives were prepared from 2-iodoanilines or2-bromoanilines reacted with alkynes following the modified method reported byZhao and co-workers.1To a solution of 2-alkynylaniline (1.00 mmol) inCH2Cl2 (8 mL) were added pyridine (5.00 mmol) and TsCl (1.20mmol) respectively. The resulting reaction mixture was stirred at rt for 8 h.After which the reaction mixture was quenched by H2O (10 mL), andthe aqueous layer was extracted with CH2Cl2 (3¡Á15 mL).The combined organic layers were dried over Na2SO4,filtered, and concentrated under reduced pressure. The crude product waspurified by silica gel flash column chromatography to obtain corresponding product.

The synthetic route of 4-Chloro-2-(phenylethynyl)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Yin-Long; Li, Jian; Yu, Sheng-Nan; Wang, Ji-Bo; Yu, Yan-Min; Deng, Jun; Tetrahedron; vol. 71; 43; (2015); p. 8271 – 8277;,
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Electric Literature of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

29.3 g (100.0 mmol) of Compound 1-A, 10.3 g (45.5 mmol) of Compound 1-B, 2.5 g (2.7 mmol) of Pd2(dba)3, 1.2 g (5.5 mmol) of PtBu3 (50 percent (%) solution in toluene), 26.2 g (272.7 mmol) of NaOtBu were mixed with 1,000 milliliters (mL) of toluene under a nitrogen (N2) atmosphere, followed by stirring under reflux to allow a reaction to occur for 12 hours. At room temperature, an organic layer was separated therefrom using water and ethyl acetate, and the solvent was dried. Then, through silica gel column chromatography, 19.0 g of Compound 1-C was obtained at a yield of 60%. [0296] MS (MALDI-TOF) m/z: 695 [M]+

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

Reference:
Patent; Samsung Display Co., Ltd.; KIM, Myeongsuk; YE, Jimyoung; YOO, Byeongwook; JEONG, Jaeho; (102 pag.)US2020/98991; (2020); A1;,
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Chlorides – an overview | ScienceDirect Topics