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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C4H6Cl2

General procedure: In the initial mixed solution prepared in the round flask in Example 1, 3-chloro-2-(chloromethyl)prop-1-ene(50 [mu] L, 0.47 mmol)By following the same procedure as in Example 1 except for using 1-pyrene methanol (240 mg, 1.03 mmol)Experiments were conducted to obtain a solid state of the compound containing pyrene dimer, 120 mg in 49% yieldOctane-1,8-diol (99 mg, 0.68 mmol) (1 eq.)And 1-(bromomethyl)pyrene (440 mg, 1.49 mmol) (2.2 eq.),3 mL ([diol] = 50 mM) in anhydrous dimethylformamide in (DMF)To room temperature in the presence and condition of N2 and NaH (3 eq.), It was added to the round bottom flask. The mixed solution in the flask was stirred at room temperature for 1 hour.After that,Then quenched and diluted with distilled water was added to the solution.next, The organics were extracted by the addition of methyl-dichloro (DCM) to the mixed solution,The resulting organic layer was again distilled under reduced pressure to reotgo so that solution filtered through a filter containing sodium sulfate (Na2SO4).The resultant was purified by silica gel column chromatography (EtOAc: Hexane = 1: 5 (volume ratio)) of the solid state compound containing pyrene dimer increasing the purity of the resultant using,To give the 120 mg at a yield of 31%.

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 1871-57-4.

Reference:
Patent; Inha UniversityIndustry-AcademicCooperation Foundation; Jo, Dong Gyu; (29 pag.)KR101542140; (2015); B1;,
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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. 4152-90-3, name is (3-Chlorophenyl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 4152-90-3

Compound (E) (12.5 g, 45.9 mmol) prepared in the step 4 was dissolved in tetrahydrofuran (400 mL), then triethylamine (19.2 ml, 3 equivalents) and 3-chlorobenzylamine (11.2 mL, 2 equivalents) were added and the mixture was stirred at 40°C for 20 hours. The salt separated out therefrom was removed by filtration and the solvent was evaporated. The residue was purified by a chromatography (chloroform:methanol = 100:1 –> 40:1) and a mixed solvent of hexane/ethyl acetate (3:1) was added to a concentrated residue of a fraction containing the objective substance so that the crystals were separated out. The suspension containing the crystals was stirred for 1 hour and the crystals separated out therefrom were filtered and dried in vacuo to prepare compound (F) (11.9 g, yield: 69percent).

According to the analysis of related databases, 4152-90-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; KYOWA HAKKO KOGYO CO., LTD.; EP1547616; (2005); A1;,
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Synthetic Route of 622-86-6, 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 622-86-6 as follows.

5.23mL of 1-(2-chloroethoxy)benzene (38.45mmol), previously distilled on CaH2, were dissolved in 50mL of dry THF to give a colorless solution. 25mL of a solution 2M of sodium cyclopentadienide in THF were added drop-wise at -78C. The solution was warmed up to room temperature and left stirred overnight to give a white precipitate and a dark pink solution. Afterwards the mixture was quenched with methanol and cold water. The organic product was extracted by 3x 50mL ether fraction. The solution was dried over magnesium sulphate and had its solvent removed at reduced pressure to yield a brown oil (yield 89%). 1H NMR (300MHz, CDCl3) delta 2.88 [t, 2H, C5H5-(CH2CH2OC6H5),], 4.14 [t, 2H, C5H5-(CH2CH2OC6H5)], 3.01-3.20 [m, 1H, C5H5-(CH2CH2OC6H5)], 6.17-6.52 [m, 4H, C5H5-(CH2CH2OC6H5)], 6.92-7.32 [m, 5H, C5H5-(CH2CH2OC6H5)]. 13C NMR (75MHz, C6D6) delta 30.1 [C5H5-(CH2CH2OPh)], 67.8 [C5H5-(CH2CH2OPh)], 44.1 [C5H5-(CH2CH2OPh)], 114.8, 120.9, 128.1, 129.7, 134.4, 134.9, 159.1 [C5H5-(CH2CH2OPh)]. Mass (GC-MS): 186.1 [M]+.

According to the analysis of related databases, 622-86-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Saturnino, Carmela; Sirignano, Esther; Botta, Antonio; Sinicropi, Maria Stefania; Caruso, Anna; Pisano, Assunta; Lappano, Rosamaria; Maggiolini, Marcello; Longo, Pasquale; Bioorganic and Medicinal Chemistry Letters; vol. 24; 1; (2014); p. 136 – 140;,
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Application of 1005-56-7,Some common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, molecular formula is C7H5ClOS, 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 alcohol 12 (150 mg, 0.288 mmol), pyridine (93 muL, 1.15 mmol) and DMAP (3.5 mg, 29 mumol) in dry CH2Cl2 (28 mL) was added phenyl chlorothionoformate (80 muL, 0.576 mmol) at room temperature. After being stirred at 40 C for 2.5 h, the reaction mixture was poured into H2O (60 mL). The mixture was extracted with AcOEt (50 mL x3). The combined organic layer was washed with brine (100 mL), and dried over anhydrous Na2SO4. The solution was concentrated to dryness in vacuo. The residue was purified by flash column chromatography (silica gel 4 g, AcOEt/hexane 1:9?1:4) to give phenyl thiocarbonate S1 (178 mg, 94%) as a white solid.

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

Reference:
Article; Adachi, Masaatsu; Sakakibara, Ryo; Satake, Yoshiki; Isobe, Minoru; Nishikawa, Toshio; Chemistry Letters; vol. 43; 11; (2014); p. 1719 – 1721;,
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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 4584-46-7 as follows. Application In Synthesis of 2-Chloro-N,N-dimethylethanamine hydrochloride

Caesium carbonate (3.0 Eq), sodium iodide (0.14 Eq) and 2-chloro-N,N- dimethylethylamine hydrochloride (1.5 Eq) are added to a suspension of p-bromo-phenol (1.0 Eq) in butanone (50 mL). The suspension is kept under reflux for four hours, after which the solid is filtered through a Hirsch funnel and washed with acetone, and the solvent is evaporated at low pressure. The crude product (yellow oil) is purified by silica-gel chromatography (eluent: dichloromethane-methanol; 95:5) to obtain the desired product (2-p-bromophenoxyethyl-N,N-dimethylamine) as a colourless oil (yield 70%).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITA’ DEGLI STUDI DI MILANO; FUMAGALLI, Laura; PICOZZI, Claudia; REGAZZONI, Luca; CARINI, Marina; ALDINI, Giancarlo; VISTOLI, Giulio; (26 pag.)WO2019/53626; (2019); 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. 622-86-6, name is (2-Chloroethoxy)benzene, A new synthetic method of this compound is introduced below., SDS of cas: 622-86-6

Example 29 N-2-(4-(2-phenoxyethoxy)-phenyl)-propyl-2-propanesulfonamide. To a stirred mixture of N-tertbutoxyacetyl-2-(4-hydroxyphenyl)propyl-2-propanesulfonamide (0.250 g,.70 mmol) in dry dimethylformamide (4 mL) was added sodium hydride (0.062 g, 0.87 mmol) under nitrogen. The resulting mixture was stirred 30 minutes at ambient temperature or until hydrogen gas evolution had ceased. Next, beta-chlorophenetole (0.120 g, 0.77 mmol) and sodium iodide (0.042 g, 0.25 mmol) are added and the resulting mixture was heated to 65C for 12 h. The resulting mixture was cooled and partitioned between ethyl acetate and water. The organic layer was washed with water (2 X 20 mL) and brine (1 X 20 mL), dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo followed by chromatography on silica gel eluding with ethyl acetate-hexane gave 0.250 g (75%) of the protected sulfonamide. To a stirred mixture of dichloromethane: trifluoroacetic acid (2 mL, 1:1) was added the protected sulfonamde (0.220 g, 0.42 mmol) under nitrogen. The resulting mixture was stirred at ambient temperature for 4 h. The mixture was partitioned between dichloromethane and 10% aqueous potassium carbonate. The organic layer was washed with brine (1 X 20 mL), dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo gives 0.166 g (96%) of the pure title compound. Mass Spectrum: MS +1= 378.5

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; ELI LILLY AND COMPANY; EP994110; (2000); A1;,
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These common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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. SDS of cas: 2533-69-9

Step 1-Synthesis of 4-[6-bromo-2-(trichloromethyl)-1,3-benzodiazol-1-yl]pyrimidin-2-amine To a solution of 4-N-(2-amino-5-bromophenyl)pyrimidine-2,4-diamine (3.0 g, 10.71 mmol) in acetic acid (10 mL) was added methyl 2,2,2-trichloroethanimidoate (1.4 mL, 11.25 mmol). The reaction was stirred at 45 C. for 7 hr. Water (15 mL) was then added. The precipitate was collected by filtration and dried under vacuum to give the title product (3.94 g as the acetic acid salt); 1H NMR (500 MHz, DMSO) delta 1.90 (3H, s), 7.01 (1H, d, J=5.0 Hz), 7.21 (2H, s), 7.75-7.46 (2H, m), 8.09-7.75 (1H, m), 8.58 (1H, d, J=5.0 Hz); LC-MS: m/z=+406/408/410/412 (M+H)+.

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

Reference:
Patent; Genentech, Inc.; US2012/214762; (2012); A1;,
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Synthetic Route of 15205-11-5, A common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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 281-[(2-Chloro-4-fluorophenyl)methyl]-4-(4-fluoro-2,6-dimethylphenyl)-2,3- piperazinedione (E28)Methyl [(4-fluoro-2,6-dimethylphenyl)(2-oxoethyl)amino](oxo)acetate (0.15 g, 0.49 mmol) was dissolved in dichloromethane (5 ml) and cooled to O0C. 4 Angstrom molecular seives (0.3 g, 0.49 mmol), acetic acid (0.09 ml, 1.48 mmol), 2-chloro-4- fluorobenzylamine (0.07 ml, 0.54 mmol) and sodium triacetoxyborohydride (0.16 g, 0.74 mmol) were added. After 5 minutes, the reaction was warmed to room temperature and stirred for 16 hours overnight. Saturated aqueous sodium bicarbonate (5 ml) was added and the mixture stirred for 10 minutes. The organic layer was separated using a hydrophobic frit and concentrated in vacuo. The crude material was purified by mass-directed automated HPLC to yield 1-[(2-chloro-4- fluorophenyl)methyl]-4-(4-fluoro-2,6-dimethylphenyl)-2,3-piperazinedione (0.083 g) as a white solid. LC/MS [M+H]+ = 379, retention time = 2.84 minutes.

The synthetic route of 15205-11-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; CHAMBERS, Laura Jane; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; STEADMAN, Jon Graham Anthony; WALTER, Daryl Simon; WO2010/125103; (2010); 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. 694-80-4, name is 1-Bromo-2-chlorobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-2-chlorobenzene

1L three bottles,To a solution of 32.5 g of 2,4,6-triisopropylbromobenzene,5.6 g of magnesium turnings and 300 mL of anhydrous THF,20 g of o-chlorobromobenzene was dropwise added,2,4,6-triisopropyl-2-bromobiphenyl Grignard reagent,Refluxed for 2 hours,Down to room temperature,2.4 g of tetrakis (triphenylphosphine) palladium was added,Stirred for 30 minutes,18.8 g of di-tert-butylphosphonium chloride was added dropwise at room temperature,The reaction was refluxed for 5 hours.And the mixture was added dropwise to the reaction solution under ice-water bath200 mL of saturated aqueous ammonium chloride was quenched,Liquid separation,The organic phase is dissolved,Add methanol crystallization,And filtered to obtain 41.7 g of white 2-di-tert-butylphosphine-2,4,6-triisopropylbiphenyl,Yield 94%.

The synthetic route of 694-80-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Panjin Gelin Kaimo Technology Co., Ltd.; Rao, Zhihua; Gong, Ningrui; (12 pag.)CN105859774; (2016); A;,
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Reference of 886762-39-6,Some common heterocyclic compound, 886762-39-6, name is 3,4-Dichloro-2-fluoroaniline, molecular formula is C6H4Cl2FN, 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.

3,4-Dichloro-2-fluoroaniline (1.8 g, 10 mmol), 2,4-dichloropyrimidine (2.25 g, 15 mmol) and hydrochloric acid (0.5 mL, 12 M) were added to 5mL of isopropyl alcohol and then put to reflux for 2h. The reaction mixture was cooled down to room temperature and then filtered to give the title intermediate (1.2 g). m/z: ESI 292.0.

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

Reference:
Patent; Ancureall Pharmaceutical (Shanghai) Co., Ltd.; SI, Jutong; WANG, Guan; YANG, Zhihe; JIANG, Meifeng; XU, Benpo; ZHOU, Chentao; (147 pag.)EP3398939; (2018); A1;,
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