Category: iodides-buliding-blocks

Related Products of 31827-94-8, A common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, molecular formula is C8H6BrIO, 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 QC-13b To a solution of (S)-1-(benzyloxycarbonyl)pyrrolidine-2-carboxylic acid (6.5 g, 26.1 mmol) in 150 mL of ethyl acetate was added triethylamine (4.0 mL, 28.7 mmol) and Example QC-13a (8.5 g, 26.1 mmol) at 0 C. The resulting mixture was stirred at room temperature overnight. The reaction mixture was filtered. The filtrate was washed with saturated sodium bicarbonate aqueous solution, and brine. The organic layer was dried with MgSO4 and concentrated. The crude product was purified by a flash chromatography (silica gel, 10-40% ethyl acetate/hexanes) to give the product as a white solid Example QC-13b (15.3 g, 85.4%). 1H NMR (500 MHz, CDCl3) delta ppm 1.87-2.01 (m, 1H) 2.01-2.16 (m, 1H) 2.22-2.42 (m, 2H) 3.44-3.58 (m, 1H) 3.59-3.71 (m, 1H) 4.45-4.58 (m, 1H) 5.04-5.50 (m, 4H) 7.27-7.38 (m, 5H) 7.53 (d, J=8.24 Hz, 1H) 7.59 (d, J=8.24 Hz, 1H) 7.85 (dd, J=8.39, 3.81 Hz, 2H). LC/MS: Anal. Calcd. for C21H21INO5 [M+H]+ 494.05; found 494.32.

The synthetic route of 31827-94-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2010/249190; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 627-32-7, 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. 627-32-7, name is 3-Iodo-1-propanol, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 4; N’-(4-(3-Hydroxypropoxy)-3-methoxybenzylidene)-3-(3-methyl-lH-indol-1 -yl)propanehydrazide; [0496] (a) 4-(3-Hydroxypropoxy)-3-methoxybenzaldehyde: To a stirred solution of vanillin (304 mg, 2 mmol) in DMF (4 rnL) at room temperature was added 3-iodo-l-propanol (0.29 mL, 3 mmol) and K2CO3 (553 mg, 4 mmol). The reaction mixture was stirred at room temperature for 7 hours followed by quenching with aq. NH4Cl. The product was extracted three times into EtOAc and the combined organic layers were dried (Na2SO4). The material was purified on silica gel using EtOAc-hexanes (0 to 70%) and to give 392 mg (93%) of the product as an off-white waxy solid.

The chemical industry reduces the impact on the environment during synthesis 3-Iodo-1-propanol. I believe this compound will play a more active role in future production and life.

Reference:
Patent; STEIN, Philip; DAINES, Robert; SPROUS, Dennis; O’GRADY, Harold; WO2010/132615; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3930-83-4,Some common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, molecular formula is C7H6INO, 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.

At room temperature,A reaction tube equipped with a stirring magnet was charged with 0.2 mmol of the compound represented by the formula (I-2)0.005 mmol catalyst Dichloro (p-cymene) ruthenium dimer ([RuCl2 (cymene)] 2),0.24 mmol cesium acetate,Then purged with nitrogen,Under nitrogen protection was added 1mL isopropanol,Stirring heated to 100 ,And reacted at this temperature for 20h.After the reaction,The reaction solution was cooled to room temperature,Filtration with a layer of silica gel funnel,Then, the solvent was distilled off under reduced pressure,The residue was purified by flash column chromatography (petroleum ether / ethyl acetate,Both volume ratio of 1: 1) purification,Thus, the target dehalogenation product represented by formula (III-2) was obtained.Calculated,The yield is 98%.

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

Reference:
Patent; Wenzhou University; Xia Yuanzhi; You Tingjie; (11 pag.)CN106588687; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 90347-66-3, A common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, molecular formula is C9H9IO2, 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.

Methyl 3-iodo-4-methylbenzoate (SM1) (30 g, 0.471 mol) was dissolved in tetrahydrofuran (1200 mL). plusTrimethylsilylacetylene (92.3 g, 0.942 mol) and diisopropylethylamine (72.9 g, 0.565 mol) were added. System vacuum,Then fill with nitrogen. Cuprous iodide (8.92 g, 0.047 mol) and bistriphenylphosphinepalladium dichloride (16.5 g, 0.024 mol) were added.The system is evacuated and filled with nitrogen. After stirring at 80 C for 4 hours under a nitrogen atmosphere and cooling to room temperature, the mixture was filtered through celite and the celite washed thoroughly with ethyl acetate. The filtrate was washed with water and brine, dried over sodium sulfate, filtered and concentrated to dryness. The crude product was purified by column chromatography (ethyl acetate / petroleum ether = 1: 50) to give the title compound (95.1 g, 82.6%) as a brown solid.

The synthetic route of 90347-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Life Sciences Institute; Zhang Zhiyuan; Huang Shaoqiang; Ren Yan; Cui Bo; Cao Weiye; Liu Chunyan; Liu Xiao; (27 pag.)CN107353286; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene, 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. Formula: C7H6INO3

2-Iodo-5-methoxy-N-(4-methoxybenzyl)aniline (7f): 12 Iron (1.68 g, 30.0 mmol)was added in one portion to a stirred solution of NH4Cl (2.67 g, 500 mmol) in H2O(50 mL), and the resulting suspension was stirred at rt for 5 min. A solution of 1-iodo-4-methoxy-2-nitrobenzene (2.79 g, 10.0 mmol) in EtOH (100 mL) was then added, the resulting mixture was slowly warmed up to 60 C, and stirring was continued at this temperature for 2 h. The reaction mixture was filtered through a short pad of Celite, and the filtrate was extracted with EtOAc (3 × 50 mL). The combined organic fractions were washed with brine (100 mL), dried over anhydrous Na2SO4 and concentrated to give crude 2-iodo-5-methoxyaniline (2.35 g) as a brown oil, which was used in the next step without additional purification. From this material and 4-methoxybenzaldehyde (1.28 g, 9.44 mmol), compound 7f (2.89 g, 78% overtwo steps) was obtained according to GP1b as a colorless oil, which spontaneously crystallized when stored in a freeze

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

Reference:
Article; Rassadin, Valentin A.; Scholz, Mirko; Klochkova, Anastasiia A.; De Meijere, Armin; Sokolov, Victor V.; Beilstein Journal of Organic Chemistry; vol. 13; (2017); p. 1932 – 1939;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C3H4F3I

110 g (760 mmol) of thiobarbituric acid of formula (XI) was added to 360 mL of water at room temperature,System was suspended state,66.9 g (1.67 mol) of sodium hydroxide was added to the system,The system gradually become clear,Plus,Stir at room temperature for 0.5 h.To the system was added 220 ml of N, N-dimethylformamide,Then 340.4 g (1.52 mol) of 1-iodo-3,3,3-trifluoropropane was added to the system,Plus,Heating to 60 C stirring reaction 8h,TLC monitoring to the basic disappearance of raw materials,The reaction is complete,Stop the reaction,Cooling to room temperature,With 2mol / L hydrochloric acid to adjust the pH to 2.5,filter,Washed cake,After solid drying,Beating,Filtered to give 171.5 g of a white solid,I.e. a compound of formula (X)Yield: 94%

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shandong Bainuo Pharmaceutical Co., Ltd.; Zhen Yizhan; Zhang Zhiqiang; Gao Changsong; Lv Wei; Zhang Zhen; (19 pag.)CN105061431; (2017); B;,
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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C3H4F3I

[0265] A solution of Mg (1.16 g, 1.6 eq.) and I2 (cat.) in Et2O (48 mL) was treated with 3,3,3-trifluoro-1-iodopropane (8.0 g, 1.2 eq. initially 20% of total) and the resulting solution was heated to reflux to initiate Grignard formation. Following initiation, the remaining 3,3,3-trifluoro-1-iodopropane was added dropwise to maintain a gentle reflux. The reaction mixture was stirred at room temperature an additional hour and transferred via canulae to a solution of 4-trifluorobenzaldehyde (4.1 mL, 30 mmol) in Et2O (95 mL) at 0 C. The resulting solution was stirred at 0 C. for 1 hour and room temperature for 1 hour. The reaction was quenched by pouring it over ice (100 g) and saturated NH4Cl. The resulting solution was extracted with CH2Cl2, the combined organics were dried over Na2SO4, filtered, concentrated and used without further purification.

According to the analysis of related databases, 460-37-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Schering Corporation; US2003/232837; (2003); 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. 135050-44-1, name is 3-Chloro-4-iodoaniline, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

Ethyl 3-(5-(2-(bromomethyl)-4,5-difluorophenyl)picolinamido)propanoate (1.0 g, 2.3 mmol), 3-chloro-4-iodoaniline (1.2 g, 4.7 mmol), and K2CO3 (647 mg, 4.7 mmol) were diluted with DMF (2.4 mL) and the resulting mixture was stirred at room temperature. After 2 h the resulting mixture directly purified via column chromatography to yield the title compound.

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; Chakravarty, Devraj; Kreutter, Kevin; Powell, Mark; Shook, Brian; Song, Fengbin; Xu, Guozhang; Yang, Shyh-Ming; Zhang, Rui; Zhao, Bao-Ping; US2012/302610; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 32024-15-0, COA of Formula: C9H9IO3

To a mixture of N-(tert-butyl)hydroxylamine hydrochloride (S3) (930 mg, 7.44 mmol), 3-iodo-4,5-dimethoxybenzaldehyde (S4) (3.27 g, 11.2 mmol, 1.50 equiv), triethylamine (2.06 mL, 14.9 mmol, 2.00 equiv), and MgSO4 (4.46 g, 37.2 mmol, 5.00 equiv) were added toluene (100 mL) at room temperature and the mixture was refluxed with stirring for 3 days. After cooling to room temperature, to the mixture was added water (50 mL) and the mixture was extracted with EtOAc (50 mL × 3). The combined organic extract was washed with aqueous saturated solution of sodium bicarbonate (20 mL), brine (20 mL), dried (Na2SO4),and after filtration, the filtrate was concentrated under reduced pressure. The residue was purified by flash column chromatography (silica-gel 70.0 g, n-hexane/EtOAc = 10/1) to give N-tert-butyl(3-iodo-4,5-dimethoxybenzylidene)amine N-oxide (9) (1.69 g, 4.66 mmol, 62.6%) as a colorless solid.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Iodo-4,5-dimethoxybenzaldehyde, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yoshida, Suguru; Uchida, Keisuke; Hosoya, Takamitsu; Chemistry Letters; vol. 44; 5; (2015); p. 691 – 693;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 328-73-4,Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, 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.

N-Methyl-2-pyrrolidone (10 mL) was added to 4-bromothiophenol (0.500 g, 2.64 mmol) in a sealed tube and the mixture was purged with argon for 5 minutes. After this time, 3,5-bis(trifluoromethyl)iodobenzene (0.89 g, 2.64 mmol), CuCl (0.131 g, 1.32 mmol), tetramethyl heptanedione (0.14 mL, 0.66 mmol) and cesium carbonate (1.70 g, 5.28 mmol) were added to the reaction mixture. The reaction mixture was stirred at 130° C. under argon for 2 hours. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, and filtered through a celite bed. The filtrate was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to yield the crude product. Silica gel chromatography (neat hexanes) provided impure 1-(4-bromo-phenylsulfanyl)-3,5-bis(trifluoromethyl)benzene (0.44 g). MS calcd. for C14H8BrF6S [(M+H)+] 402, obsd. 402.

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; Firooznia, Fariborz; Lin, Tai-An; Mertz, Eric; So, Sung-Sau; Sidduri, Achyutharao; Tilley, Jefferson Wright; US2013/225588; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com