Tag: M.W=200-300

Application of 19718-49-1, A common heterocyclic compound, 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, molecular formula is C8H8INO2, 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.

A solution of methyl 4-amino-3-iodobenzoate (1.0 g, 3.61 mmol) and triethylamine (1.003 mL, 7.22 mmol) in dichloromethane (20 mL) was added dropwise to a cooled (0 0C) solution of trifiuoroacetic anhydride (1.275 mL, 9.02 mmol) in dichloromethane (5 mL). The cooling was removed, the mixture was stirred at room temperature for 3 hours, poured into ice-water and extracted with dichloromethane. The organic phase was dried over sodium sulfate and the solvent was evaporated. Purification by column chromatography, using heptane/ethyl acetate (4:1) as the eluent, gave 1.23 g (91% yield) of the title compound. 1H NMR (500 MHz, CD3OD) delta ppm 8.54 (d, 1 H) 8.07 (dd, 1 H) 7.57 (d, 1 H) 3.93 (s, 3 H); MS (ESI) m/z 372 [M-I]”.

The synthetic route of 19718-49-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2009/64251; (2009); A1;,
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Reference of 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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.

General procedure: A 50mL round-bottomed flask equipped with a gas inlet tube, a reflux condenser, and a magnetic stirring bar was charged with MCM-41-S-PdCl2 (173mg, 0.05 mmol Pd), aryl halide (5.0 mmol) and HCOONa (7.5 mmol). The flask was flushed with carbon monoxide. DMF (5 mL) was added by syringe and a slow stream of CO was passed into the suspension. The mixture was vigorously stirred at 100-110C for 4-24h, cooled to room temperature, and diluted with diethyl ether (50 mL). The palladium catalyst was separated from the mixture by filtration, washed with distilled water (2×10 mL), ethanol (2×10 mL) and ether (2×10 mL) and reused in the next run. The ethereal solution was washed with water (3×20mL) and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (hexane-ethyl acetate=10:1). (0008) All formylation products were characterized by comparison of their spectra and physical data with authentic samples. IR spectra were determined on a Perkin-Elmer 683 instrument. 1H NMR (400MHz) and 13C NMR (100MHz) spectra were recorded on a Bruker Avance 400MHz spectrometer with TMS as an internal standard and CDCl3 as solvent.

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hao, Wenyan; Ding, Guodong; Cai, Mingzhong; Catalysis Communications; vol. 51; (2014); p. 53 – 57;,
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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. 77317-55-6, name is Methyl 2-amino-5-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C8H8INO2

A solution of methyl 2-amino-5-iodobenzoate (7.02 g, 25.3 mmol) and 2-(tetrahydro-2H-pyran-4-yl)acetic acid (3.76 g, 26.1 mmol) in pyridine (25 mL) was stirred at ?-40 C. under argon while POCl3 (2.58 g, 27.8 mmol) was added dropwise over 3 minutes. The cold bath was immediately removed and the reaction was allowed to stir for 1 hour. The reaction was then diluted with water (75 mL) and extracted with DCM (75 mL). The combined orange organic layers were washed with 6 M aqueous HCl (50 mL), 1 M aqueous HCl (50 mL), and 2 M aqueous K3PO4 (50 mL), dried (Na2SO4), filtered, and concentrated to provide the title compound as an orange solid.

According to the analysis of related databases, 77317-55-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JOHNSON & JOHNSON; LEONARD, KRISTI A.; BARBAY, KENT; EDWARDS, JAMES P.; KREUTTER, KEVIN D.; KUMMER, DAVID A.; MAHAROOF, UMAR; NISHIMURA, RACHEL; URBANSKI, MAUD; VENKATESAN, HARIHARAN; WANG, AIHUA; WOLIN, RONALD L.; WOODS, CRAIG R.; FOURIE, ANNE; XUE, XIAOHUA; CUMMINGS, MAXWELL D.; MCCLURE, KELLY; TANIS, VIRGINIA; US2015/111870; (2015); A1;,
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Application of 21304-38-1, 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. 21304-38-1, name is 4-Iodobenzene-1,2-diamine belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4-iodo-1,2-phenylenediamine (2 g, 1 eq), 4-dimethylaminonitrozoaniline (1.26 g, 1 eq) and NaOH (340 mg, 1 eq) were mixed neat and heated at 70 C. for 20 min with constant triturating. The resulting paste was extracted with toluene, concentrated in vacuum and purified by flash chromatography (SiO2, hexane/AcOEt, 8/2) giving a mixture of two isomers (3 and 4 iodo) as a red solid in 32% yield; 4-iodo-1,2-phenylenediamine (2 g, 1 eq), 4-dimethylaminonitrozoaniline (1.26 g, 1 eq) and NaOH (340 mg, 1 eq) were mixed neat and heated at 70 C. for 20 min with constant triturating. The resulting paste was extracted with toluene, concentrated in vacuum and purified by flash chromatography (SiO2, hexane/AcOEt, 8/2) giving a mixture of two isomers (3 and 4 iodo) as a red solid in 32% yield.

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

Reference:
Patent; Tamagnan, Gilles D.; Alagille, David; Costa, Herve Da; US2007/258887; (2007); 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. 127654-70-0, name is 1-Chloro-3-fluoro-2-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H3ClFI

70.00 g (1.0 eq) of 2-bromo-9H-carbazole and 52.14 g (1.5 eq) of KOtBu were placed in 1.0 L of DMF (dimethylformamide) and heated and stirred. At the start of the reflux, 80.23 g (1.1 eq) of 1-chloro-3-fluoro-2-iodobenzene was added. After the reaction was completed after 3 hours, the reaction was poured into water and the crystals were dropped and filtered.The filtered solid was completely dissolved in CHCl3, washed with water, and again decompressed to remove the solvent, which was purified by column chromatography. 107.3 g (yield 78%) of the compound of the formula 1-a was obtained.

According to the analysis of related databases, 127654-70-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LG Chem, Ltd.; Lee Jeong-ha; Park Tae-yun; Cho Seong-mi; Kim Min-jun; (118 pag.)KR101891031; (2018); B1;,
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Synthetic Route of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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.

14.4: (3-iodo-benzyl)-dimethyl-amine To a cold (0 C.) solution of 3-iodo-benzaldehyde (3 g, 12.9 mmol) in anhydrous dichloromethane (130 ml) were added acetic acid (1.9 ml) and N,N-dimethylacetamide. The yellow solution is stirred 10 minutes at 0 C. and sodium triacetoxyborohydride (6.85 g, 32.33 mmoles) is added by portions. The resulting mixture is stirred at room temperature for 90 minutes and evaporated to dryness under reduced pressure. Ethyl acetate and a saturated aqueous hydrogen carbonate solution were added to the residue and the two layers were separated The organic phase was washed with water, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum to yield (3-iodo-benzyl)-dimethyl-amine (3.05 g, 90%) as a brown oil. LC/MS (Method LC8): Rt=0.86 min; m/z=262 [M+H]+.

The synthetic route of 696-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI; LOEHN, Matthias; MENDEZ-PEREZ, Maria; PFEIFFER-MAREK, Stefania; KANNT, Aimo; BEGIS, Guillaume; DUCLOS, Olivier; JEANNOT, Federic; US2013/65894; (2013); 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. 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 2401-21-0

EXAMPLE 45 A solution of 5-aminospiro[benzo[b]furan-2(3H),1′-cyclopropane]-3-one (0.181 g.) and pyridine (0.083 mg.) in tetrahydrofuran (5 ml.) was cooled to -17° C. To the solution was added dropwise iodobenzenedichloride (0.282 g.), which had been prepared by conventional method, dissolved in tetrahydrofuran (1.5 ml.) over 50 minutes, followed by stirring for 1 hour. The reaction mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with water, dried and the solvent was evaporated off. The residue was subjected to column-chromatography, using chloroform as the eluent. The first fraction was concentrated under reduced pressure to remove the solvent. By the above procedure, there was obtained 5-amino-4-chlorospiro[benzo[b]furan-2(3H),1′-cyclopropane]-3-one as yellow crystals. Yield 0.038 g. Mass spectrum: C12 H12 O2 NCl, molecular ion peak (209).

The synthetic route of 2401-21-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US4284644; (1981); A;,
Iodide – Wikipedia,
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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 16932-44-8 as follows. Safety of 2-Iodo-1,3-dimethoxybenzene

The compound (B142, 5g18.9mmol) obtained above was dissolved in the drying THF, andthe mixture obtained by adding gradually the THF solution (9.5 mL, 2.0 M19.0mmol) ofisopropyl MAGUNE SIMM chloride at 50 degree C was stirred at the room temperature for 1hour.Next, the mixture was cooled at 78 degree C, and the phosphorus trichloride (1.3 g,9.5mmol) was added slowly. Then, the reaction intermediate containing the bis(2,6dimethoxyphenyl)phosphine chloride (B-14-4) obtained by stirring all night at the roomtemperature was used for the next reaction, without refining.

According to the analysis of related databases, 16932-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JAPAN POLYETHYLENE CORPORATION; JAPAN POLYPROPYLENE CORPORATION; XIN, SHIXUAN; SHIMIZU, FUMIHIKO; SATO, NAOMASA; TANNA, AKIO; (45 pag.)JP5812764; (2015); B2;,
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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 101335-11-9 as follows. Formula: C6H3ClFI

Step 1. Ethyl 2-(4-(2-chloro-4-fluorophenyl)-4-hydroxycyclohexyl)acetate. A solution of n-butyllithium in hexanes (1.6 M, 81.4 mL, 130 mmol) was added dropwise to a solution of 2- chloro-4-fluoro-l-iodobenzene (16.6 mL, 130 mmol) in tetrahydrofuran (197 mL) at -78C. The reaction mixture was allowed to stir at -78C for 1 h before the addition of ethyl 2-(4- oxocyclohexyl)acetate (19.2 mL, 109 mmol) in one portion. The reaction was allowed to warm to room temperature and stirred at room temperature for 1 h. The reaction was quenched with a saturated solution of ammonium chloride (500 mL) and extracted with EtOAc (3 x 150 mL), combined organics dried (Na2S04) and concentrated under reduced pressure. The residue was purified by flash chromatography on silica, eluting with 0-40% EtOAc in hexanes to yield the product as a colorless oil (26.7 g, 78%). 1H NMR (400 MHz, CDCb) d 7.65 (dd, / = 8.86, 6.30 Hz, 1H), 7.21 – 7.09 (m, 1H), 7.03 – 6.94 (m, 1H), 4.27 – 4.07 (m, 5H), 2.62 – 2.47 (m, 2H), 2.46 – 2.18 (m, 10H), 2.15 – 1.82 (m, 6H), 1.78 – 1.34 (m, 7H), 1.34 – 1.22 (m, 7H). [M-H2O+H] = 283.1.

According to the analysis of related databases, 101335-11-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DART NEUROSCIENCE, LLC; BASINGER, THOMPSON, Jillian; BOOKSER, Brett; BURLEY, Scott; GARCIA-REYNAGA, Pablo; HUDSON, Andrew; PETERS, Marco; PRATT, Benjamin; THOMPSON, Aaron; TRAN, Joe; VALDEZ, Lino; (211 pag.)WO2019/168866; (2019); A1;,
Iodide – Wikipedia,
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Related Products of 33348-34-4, 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 33348-34-4 as follows.

A solution of the product of Step A (0.32 g, 1 .31 mmol) and 1 M NaN(SiMe3)2 in THF (2.62 ml) in anhydrous THF (2 ml) was stirred at ~-5C for 30 min under N2. To it acetyl chloride (0.1 1 ml, 1 .44 mmol) was and the mixture was stirred overnight at room temperature, than evaporated to dryness under reduced pressure. The residue was diluted to 50 ml with EtOAc, washed with H20, brine, dried over anhydrous MgS04, filtered and the filtrate evaporated to dryness. The residue was purified by crystallization from MeOH to give the title compound (0.26 g, 70%), as colourless solid. 1 H NMR (CDCI3) 8.46 (d, 1 H, J = 9 Hz), 8.03 (s, 1 H), 7.58 – 7.63 (m, 2H), 2.27 (s, 3H).

According to the analysis of related databases, 33348-34-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AKAAL PHARMA PTY LTD; GROBELNY, Damian W; GILL, Gurmit S; WO2014/63199; (2014); A1;,
Iodide – Wikipedia,
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