Month: September 2021

Reference of 141738-80-9,Some common heterocyclic compound, 141738-80-9, name is 3-Chloro-4-iodobenzotrifluoride, molecular formula is C7H3ClF3I, 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 vial was charged with N-(2,4-dimethoxybenzyl)-l-methyl-3-(4,4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yl)-N-(l,2,4-thiadiazol-5-yl)-lH-indole-6-sulfonamide (.500 g, 0.876 mmol), potassium phosphate (0.651 g, 3.07 mmol), and bis(tri-t- butylphosphine)palladium(O) (0.045 g, 0.088 mmol). The vial was flushed with Ar, then 1 ,4-dioxane (6.57 ml) and water (2.191 ml) were added in sequence, followed by 2- chloro-l-iodo-4-(trifluoromethyl)benzene (0.426 ml, 2.63 mmol). The vial was sealed and stirred at room temperature for two hours. The reaction was diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were washed with brine, dried with sodium sulfate, filtered and concentrated. The material was purified via column chromatography (RediSep Gold (Teledyne Isco, Lincoln, NE) 40g, gradient elution 0-100% EtO Ac/Heptane) to afford 3- (2-chloro-4-(trifluoromethyl)phenyl)-N-(2,4-dimethoxybenzyl)-l-methyl-N-(l ,2,4- thiadiazol-5-yl)-lH-indole-6-sulfonamide (0.405 g, 0.650 mmol, 74.2 % yield) as a light yellow solid, m/z (ESI) 624.0 (M+H)+.

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

Reference:
Patent; DINEEN, Thomas; MARX, Isaac, E.; NGUYEN, Hanh, Nho; WEISS, Matthew; AMGEN INC.; WO2013/25883; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, A new synthetic method of this compound is introduced below., SDS of cas: 355-43-1

In reaction kettleF (CF2) 6-I(1298.5 kg, 2.911 kmol)Was stirred and stirred.Next, Parroyl IPP[Half-life temperature: 40.3 C]AE-3000 so that 20% by massSolution dissolved in (1,1,2,2-tetrafluoroethyl-2,2,2-trifluoroethyl ether)(17.0 kg, 0.017 kmol)And CH2 = CHCH2 (CH2) 5H (336.5 kg, 2.999 kmol)It was dripped at the said reaction kettle.During dripping,The internal temperature was kept at 88-100 C.After completion of drippingKeep the internal temperature at 90-100 C,As a result of analyzing the reaction crude liquid A1 obtained by further stirring for 0.5 hour or more by gas chromatography,It was confirmed that F (CF2) 6CH2CHICH2 (CH2) 5H was contained.From the obtained reaction crude liquid A1,Under reduced pressure (-0.093 kPaG.Less than,Gauge pressure,?G? is added after ?kPa? or ?MPa?. )AE-3000 and excessCH2 = CHCH2 (CH2) 5HIs distilled off,Reaction solution 1a containing F (CF2) 6CH2CHICH2 (CH2) 5H(1622.4 kg) was obtained.

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; AGC glass company; Maeda, Yutaka; Mitsui, Yoshiyuki; Yamane, Shingo; (11 pag.)JP2019/108319; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 811842-30-5, These common heterocyclic compound, 811842-30-5, name is 2-Bromo-1-fluoro-4-iodobenzene, 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 mixture of 2-bromo-1-fluoro-4-iodobenzene (3.01 g, 10 mmol), Example 35a (1.472 g, 10.50 mmol), and cesium carbonate (3.42 g, 10.50 mmol) in dimethylsulfoxide (20 mL) was heated at 110 C overnight. After cooling to ambient temperature, the reaction mixture was partitioned between water and ethyl acetate. The aqueous layer was extractedwith additional ethyl acetate twice. The combined organic layers were washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was purified by column chromatography on silica gel eluting with heptanes to give the title compound (3.21 g, 76% yield) as a white solid.

The synthetic route of 811842-30-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBVIE INC.; ABBVIE PHARMACEUTICAL TRADING (SHANGHAI) CO., LTD.; FIDANZE, Steven D.; HASVOLD, Lisa A.; LIU, Dachun; MCDANIEL, Keith F.; PRATT, John; SCHRIMPF, Michael; SHEPPARD, George S.; WANG, Le; LI, Bing; (191 pag.)WO2017/177955; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., Safety of 4-Bromo-1-iodo-2-nitrobenzene

Intermediate M2-b (4.8 g, 15 mmol),2-Iodo-5-bromonitrobenzene (5.9 g, 18 mmol), sodium tert-butoxide(2.9g, 30mmol), toluene 50mL, nitrogen protection,0.17 g of Pd2(dba)3, tri-tert-butylphosphine(11ml, 10% toluene solution), stirring turned on,Heated to 100 C reflux, reaction 12h, the reaction solution washed,The organic phase was concentrated and passed through a silica gel column. The eluent was petroleum ether:Ethyl acetate = 50:1, concentrated rinse,Intermediate M2-c (6.6 g, 84.6% yield) was obtained.

According to the analysis of related databases, 112671-42-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Xing Qifeng; Zhang Wei; Zhang Xianghui; (38 pag.)CN107880049; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com