Month: March 2021

Adding a certain compound to certain chemical reactions, such as: 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, 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 672-57-1, COA of Formula: C7H3ClF3I

General procedure: A mixture of 2-(3,5-dichloro-pyridin-4-yl)-7-ethynyl-4,4-dimethyl-1,4-dihydro-chromeno[3,4-d] imidazole 19a (0.1 g, 0.270 mmol), tetrabutylammonium fluoride (0.255 g, 0.810 mmol), dichlorobis- (triphenylphosphine)palladium (II) (15 mg, 0.021 mmol), 1-chloro-2-iodo-4-trifluoromethyl-benzene (0.125 g, 0.405 mmol) was heated in dry-DMSO (4.0 mL) at 80 C for 4-6 h. The reaction mass was quenched with water and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous sodium sulfate, concentrated under reduced pressure and purified by flash chromatography to afford compound 20a (0.06 g, 42%) as brown 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, 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Muthukaman, Nagarajan; Tambe, Macchindra; Shaikh, Mahamadhanif; Pisal, Dnyandeo; Deshmukh, Sanjay; Tondlekar, Shital; Sarode, Neelam; Narayana, Lakshminarayana; Gajera, Jitendra M.; Kattige, Vidya G.; Honnegowda, Srinivasa; Karande, Vikas; Kulkarni, Abhay; Behera, Dayanidhi; Jadhav, Satyawan B.; Gudi, Girish S.; Khairatkar-Joshi, Neelima; Gharat, Laxmikant A.; Bioorganic and Medicinal Chemistry Letters; vol. 27; 11; (2017); p. 2594 – 2601;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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: 610-97-9

General procedure: ReBr(CO)5, ReCl(CO)5, (C5H5)ReO3, Re2(CO)10, and ReCl5 were commercially available andwere used without further purification. 2-(Arylethynyl)benzoic acids were prepared by the hydoration ofcorresponding methyl esters, which were prepared by the Sonogashira coupling of methyl 2-iodobenzoateand arylethyny, 1-pentyne, 1-hexyne, ethynylcyclohexane or 3,3-dimethyl-1-butyne. Other chemicalagents were obtained commercially and were purified if necessary by distillation.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 610-97-9, its application will become more common.

Reference:
Article; Umeda, Rui; Yoshikawa, Shunya; Yamashita, Kouji; Nishiyama, Yutaka; Heterocycles; vol. 91; 11; (2015); p. 2172 – 2179;,
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. 153898-63-6, name is 2-Iodo-5-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 153898-63-6

General procedure: In a flame-dried flask, AlMe3 (2 M in toluene, 1.11 mL, 2.18mmol, 1.2 equiv) was added to dry toluene (3.0 mL) under anitrogen atmosphere. The mixture was cooled to 0 C, and the2-iodoaniline (2.0 mmol, 1.1 equiv) in dry toluene (4.0 mL) was added. The mixture was stirred for a further 5 min at 0 C. Theice bath was removed, and the mixture was stirred for 20 min atroom temperature. The mixture was cooled to 0 C again, and cyclopentene carboxylate 2b (1.82 mmol, 1.0 equiv) in drytoluene (3.0 mL) was added dropwise over 2 min to the mixture. After stirring for 10 min at 0 C, the mixture was heated to 60 C, and stirring was continued for 16 h. After cooling to room temperature, HCl (1 M, 8.0 mL) was added. (Caution: gas evolution,exotherm.) The mixture was stirred for 15 min, then water (20 mL) and EtOAc (30 mL) were added. The mixture was extracted, the organic phase was separated, and the aqueous phase was re-extracted one more time with EtOAc (30 mL). Thecombined organic phases were washed with brine and dried (MgSO4). After filtration, the solvent was removed under reduced pressure, and the crude mixture was purified by column chromatography.

According to the analysis of related databases, 153898-63-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Adeyemi, Ahmed; Wetzel, Alexander; Bergman, Joakim; Branalt, Jonas; Larhed, Mats; Synlett; vol. 30; 1; (2019); p. 82 – 88;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 16932-44-8, 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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

(2) Synthesis of intermediate 4 Intermediate 2 (5 g, 18.9 mmol) was dissolved in absolute THF, and isopropylmagnesium chloride (9.5 ml, concentration: 2M, solvent: absolute THF) was slowly added thereto at -50C, and then the resultant mixture was stirred at room temperature for 1 hour. Subsequently, said mixture was cooled to -78C, and phosphorus trichloride (1.3 g, 9.5 mmol) was slowly added. After that, the mixture was stirred at room temperature overnight, and the resultant reaction product containing intermediate 4 was used for the next reaction without further purification

The chemical industry reduces the impact on the environment during synthesis 2-Iodo-1,3-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Japan Polypropylene Corporation; Japan Polyethylene Corporation; EP2351761; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 123278-03-5, These common heterocyclic compound, 123278-03-5, name is 3-Chloro-2-iodobenzoic acid, 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.

Step B: Preparation of Ethyl 2-(3-chloro-2-iodophcnyl)acetate; [0923] 3-Chloro-2-iodobenzoic acid (8.83 g, 31 .3 mmol) was stirred in thionyl chloride (125 mL) at reflux for 2 hours. The mixture was cooled to room temperature, the thionyl chloride was removed under vacuum, and the residue was azeotroped once with toluene to give the acid chloride as a dark red solid. Trimethylsilyldiazomethane (2.0M in EtzO, 124 mmol) was added to the acid chloride, and the mixture was stirred for 5 hours at room temperature. Excess reagent was destroyed by the addition of AcOH (until bubbling stopped), and the mixture was partitioned between EtOAc and saturated NaI 1CU3. The layers were separated, and the organic layer was washed with water once, brine once, dried over anhydrous MgSO4 and concentrated in vacuo. ‘I his material was dissolved in absolute EtOH (250 m L) and silver (1) oxide (catalytic amount) was added. The mixture was heated at 8O0C for 30 minutes, cooled to room temperature, and filtered through cclite. The filtrate was concentrated and purified by flash chromatography to give 7.89 g of ethyl 2-(3-chloro-2- iodophenyl)acetate as an orange oil.

The synthetic route of 123278-03-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMGEN INC.; WO2008/76427; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 88-82-4, 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. 88-82-4, name is 2,3,5-Triiodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 25 3,5-Diiodobenzyl-n-Hexyl Carbonate Preparation of s in Table I: Using the procedure of B, Gaux and D. LeHenaff, Bull. Soc. Chem. Fr., 34, 505 (1974), 2,3,5-triiodobenzoic acid (Aldrich) was treated with lithium aluminum hydride to give 3,5-diiodobenzyl alcohol with m.p. of 136.5-140 (literature 137).

The synthetic route of 2,3,5-Triiodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lafayette Pharmacal Inc.; US4175544; (1979); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 3058-39-7, A common heterocyclic compound, 3058-39-7, name is 4-Iodobenzonitrile, molecular formula is C7H4IN, 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.

The compound 4-cyanoiodobenzene 1a (1.0 mmol) was added to the reactor in that order.DMSO (5 ml), Cs2CO3 (2.0 mmol), phenol 2a (1.2 mmol) was stirred at room temperature for 6 min.Then, it was placed in an oil bath at 80 C, and reacted for 10 hours under light. After the TLC detection reaction was completed, the reaction solution was subjected to filtration, extraction and column chromatography to obtain the objective product 4a, yield 79%.

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; China Three Gorges University; Wang Long; Liu Na; Yang Qingqing; Hu Weimin; (7 pag.)CN110156635; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 13421-00-6, A common heterocyclic compound, 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

According to the procedure reported by Yu and co-workers [3], palladium acetate (22 mg, 0.10mmol), iodobenzene diacetate (644 mg, 2.0 mmol), iodine (507 mg, 2.0 mmol), and tetrabutylammonium iodine (739 mmol, 2.0 mmol) were added to a solution of 3-chlorobenzoic acid (313 mg, 2.0 mmol) in 1,2-dichloroethane (20 mL). The mixture was heated at 100 C with stirring for 2 h and then allowed to cool to room temperature. Iodobenzene diacetate (644 mg, 2.0 mmol) and iodine (507 mg, 2.0 mmol) were added to the mixture. After stirring at 100 C for 4 h, the resulting mixture was diluted with10% sodium carbonate. The aqueous layer was separated, washed with Et2O, and then acidified with 10% HCl. The resulting mixture was extracted with EtOAc and the organic layer was dried over Na2SO4; filtered; and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/EtOAc = 4/1) to give crude 5-chloro-2-iodobenzoic acid (223 mg) as a colorless solid, which was suspended in thionyl chloride (2 mL). After stirring under reflux conditions for 2 h, the resulting mixture was concentrated under reduced pressure. The remaining thionyl chloride was removed by azeotropic distillation with benzene. The residue was dissolved in anhydrous CH2Cl2 (3 mL). To the mixture were added isopropylamine (56 mg, 0.95 mmol) and triethylamine (240 mg,2.37 mmol) at 0 C under a nitrogen atmosphere. After stirring at room temperature for 13 h, the resulting solution was diluted with EtOAc. The mixture was washed with 10% HCl, saturated aqueous NaHCO3, water, and brine; dried overNa2SO4; filtered; and concentrated under reduced pressure. The residue was purified by recrystallization from hexaneand CHCl3 to give 19 (138 mg, 21% in 3 steps) as colorless needles.

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yakura, Takayuki; Fujiwara, Tomoya; Yamada, Akihiro; Nambu, Hisanori; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 971 – 978;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 2043-57-4, A common heterocyclic compound, 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, molecular formula is C8H4F13I, 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.

(W) Synthesis of 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium 1,1,2,2-tetrafluoroethanesulfonate; 1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 ml) in a large round-bottomed flask and stirred vigorously. 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 degrees C. for 24 hours. The solvent was removed under vacuum giving 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide (30.5 g) as a waxy solid. Potassium 1,1,2,2-tetrafluoroethanesulfonate (TFES-K, 12 g) was added to reagent grade acetone (100 ml) in a separate round-bottomed flask, and this solution was carefully added to the 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide which had been dissolved in acetone (50 ml). The reaction mixture was heated under reflux for approximately 16 hours. The reaction mixture was then filtered using a large frit glass funnel to remove the white Kl precipitate formed, and the filtrate was placed on a rotary evaporator for 4 hours to remove the acetone. The oily liquid was then filtered a second time to yield the product, as shown by proton NMR.

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Harmer, Mark Andrew; Junk, Christopher P.; Vickery, Jemma; Miller, Robert; US2007/66852; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

3930-83-4, name is 2-Iodobenzamide, 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. COA of Formula: C7H6INO

General procedure: To a 10 mL reaction tube were added MCM-41-L-Proline-CuBr(135 mg, 0.1 mmol), 2-halobenzamide 1 (1.0 mmol), benzylamine derivative 2 (2.0 mmol), K2CO3 (3.0 mmol), and DMSO (3 mL). The reaction mixture was stirred at 110 or 120 C under air for 6-12 h.After being cooled to room temperature, the reaction mixture was diluted with 20 mL of EtOAc, and filtered. The MCM-41-L-Proline-CuBr complex was washed with distilled water (2 5 mL) and ethanol (2 5 mL), and reused in the next run. The filtrate was washed with water (2 10 mL) and dried over MgSO4. After being concentrated in vacuo, the residue was purified by flash column chromatography on silica gel (petroleum ether/EtOAc 3:1 to 2:1)to afford the target product 3.

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yan, Nan; You, Chongren; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 897; (2019); p. 161 – 169;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com