Introduction of a new synthetic route about C8H7IO2

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-methylbenzoic acid, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3-Iodo-4-methyl-N-(3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)Benzamide: 3-Iodo-4-methylbenzoic acid (2.62 g, 10 mmol) was refluxed in soc2 (10 mL) for 5 1 h. The volatile components were removed on a rotavap and the residue was dissolved inbenzene (10 mL), concentrated to dryness on a rotavap and further dried under vacuum. The resulting acyl chloride was added to a solution 3-(4-methyl-IH-imidazol-I-yl)-5- (trifluoromethyl)benzenearnine (2.46 g, 10.2 mmol), N,N-diisopropylethylamine (1.56 g, 12 mmol), and a catalytic amount of DMAP in THF (20 mL). After stirring at rt for 2 h, the reaction10 was quenched with water. EtOAc was added and the layers separated. The combined organic layers were concentrated to dryness and used without purification in next step.

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-methylbenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARIAD PHARMACEUTICALS, INC.; GOZGIT, Joseph, M.; RIVERA, Victor, M.; SHAKESPEARE, William, C.; ZHU, Xiaotian; DALGARNO, David, C.; WO2013/162727; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Discovery of 2-Iodoethanol

According to the analysis of related databases, 624-76-0, the application of this compound in the production field has become more and more popular.

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 624-76-0 as follows. COA of Formula: C2H5IO

Example 396 (Z)-3-(2-Hydroxyethyl)-5-[{7-(4-methoxyphenyl)furo[3,2-c]pyridin-2-yl}methylene]thiazolidine-2,4-dione Step 1: Synthesis of 3-(2-hydroxyethyl)thiazolidine-2,4-dione Thiazolidinedione (12.8 mmol), 2-iodoethanol (15.1 mmol), potassium carbonate (17.4 mmol) and tetrabutylammonium iodide (1.3 mmol) were placed in acetone (25 ml), and stirred at 40 C. for 10 hours. The reaction mixture was cooled to room temperature, filtered through Celite, and concentrated under reduced pressure to yield brown oil. The residue thus obtained was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1, v/v) to obtain the title compound as colorless oil (yield: 54%). 1H NMR (CDCl3, 400 MHz) delta 4.00 (s, 2H), 3.85 (brs, 4H), 1.94 (brs, 1H)

According to the analysis of related databases, 624-76-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; YUHAN CORPORATION; Seo, Hyoung Sig; Kim, Tae Kyun; Lee, Hyun Joo; Kim, Dong Hoon; Lee, Gyu Jin; Park, Jun Chul; Gal, Ji Yeong; Kim, Tae-hoon; Hyun, Kwan Hoon; Ahn, Kyoung Kyu; Park, Kaapjoo; Nam, Su Youn; Lee, Ge Hyeong; Lim, Hee Jong; US2015/191478; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

New downstream synthetic route of C7H4FIO2

The synthetic route of 4-Fluoro-2-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 56096-89-0, name is 4-Fluoro-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. Recommanded Product: 4-Fluoro-2-iodobenzoic acid

General procedure: To a stirred solution of 2-iodobenzoic acids a (10 mmol) in CH2Cl2, was added DCC (dicyclohexylcarbodiimide, 11 mmol), DMAP (Dimethylaminopyridine, 2 mmol) and alcohols b (10 mmol) in sequence. The resulting solution was stirred overnight at room temperature then filtered through a sand core funnel and washed with diethyl ether (2 x 40mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to obtain the pure product c in moderate to good yields. To a soluton of 2-iodobenzoates c in Et3N (5 mL) was added PdCl2 (PPh3)2 (4 mol %) and CuI (2 mol %) and the reaction vial was flushed with Ar and the reaction mixture was stirred for 5 minutes. A solution of propargyl alcohols d (1.05 equiv) in Et3N (5 mL) were then added dropwise through a syringe for 5 minutes. The resulting solution was stirred at room temperature overnight. When the reaction was considered complete as determined by TLC analysis, the mixture was quenched by addition of saturated aqueous ammonium chloride (10 mL) and extracted with ethyl ether (3 x 40 mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to give 1.

The synthetic route of 4-Fluoro-2-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhu, Hai-Tao; Tong, Xiao-Juan; Zhou, Ni-Ni; Yang, De-Suo; Fan, Ming-Jin; Tetrahedron Letters; vol. 57; 49; (2016); p. 5497 – 5500;,
Iodide – Wikipedia,
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Sources of common compounds: 27913-58-2

According to the analysis of related databases, 27913-58-2, the application of this compound in the production field has become more and more popular.

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 27913-58-2 as follows. HPLC of Formula: C10H11IO2

4-(p-Iodophenyl)butyric acid (580 mg, 2.0 mmol) and N-hydroxysuccinimide (345 mg, 3.0 mmol) were dissolved in CH2Cl2 (10 mL) and cooled to 0 C. under Ar. A solution of DCC (620 mg, 3.0 mmol) in CH2Cl2 (4 mL) was added dropwise over 10 min, and the reaction was warmed to rt and stirred overnight at rt. The reaction was filtered to remove the insoluble urea by-product, and the filter cake was washed with CH2Cl2. The organic fractions were combined and concentrated under reduced pressure, and the crude product was purified by silica chromatography (EtOAC:hexane=1:1) to give N-succinimidyl 4-(p-iodophenyl)butanoate as a white solid (400 mg, 52%). 1H NMR (500 MHz, CDCl3) delta 7.61 (d, 2H, J=8.2 Hz), 6.96 (d, 2H, J=8.2 Hz), 2.85 (br s, 4H), 2.68 (t, 2H, J=7.6 Hz), 2.60 (t, 2H, J=7.3 Hz), 2.04 (quint, 2H, J=7.4 Hz).

According to the analysis of related databases, 27913-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Cornell University; Babich, John W.; Kelly, James M.; Amor-Coarasa, Alejandro; Ponnala, Shashikanth; (36 pag.)US2017/368005; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Extracurricular laboratory: Synthetic route of C3H6ClI

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Application of 6940-76-7, A common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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.

3.101 1-(3-Chloropropyl)-1H-indol-2,3-dione (85LM02). A 500 ml flask was charged with 1H-indol-2,3-dione (isatin) (3.62 g, 25 mmol), 1-chloro-3-iodopropan (2.8 ml, 27 mmol) and Cs2CO3 (18 g, 55 mmol) in MeCN (200 ml). The mixture was stirred 40 C. for 48 hours. Water (50 ml) and EtOAc (50 ml) were added and the phases were separated. The aqueous phase was re-extracted with EtOAc (50 ml). The combined org. layer were dried (Na2SO4) and evaporated to dryness. The crude product was purified by to column chromatography (SiO2; EtOAc/n-heptane 1:4) to give the title compound (85LM02) (4.2 g, 80%). 1H NMR (CDCl3) delta 2.20 (qv, 2H), 3.60 (t, 2H), 3.90 (t, 2H), 7.00 (d, 1H), 7.15 (t, 1H), 7.55-7.65 (m, 2H); HPLC-MS (ammonium acetate) [M+H]+=224.2.

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACADIA Pharmaceuticals Inc.; US6951849; (2005); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Research on new synthetic routes about 3-Iodo-1-propanol

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.

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. 627-32-7, name is 3-Iodo-1-propanol, A new synthetic method of this compound is introduced below., SDS of cas: 627-32-7

E: 3-(4-Bromo-2-(trifluoromethyl)-phenoxy)propan-1-ol; 3-lodopropanol (11.23g) was added to a mixture of 4-bromo-2- (trifluoromethyl)-phenol (15g) and potassium carbonate (17.2g) in acetonitrile (150ml). The above mixture was refluxed for 4 hours then diluted with ethyl acetate (500ml) and water (300ml). Organic layer was seperated, dried over magnesium sulphate, solvent removed under reduced pressure to give expected product clean enough for use at the next step (18.6g). 1H NMR (CDCI3)delta: 7.67 (d, 1 H), 7.58 (dd, 1 H), 6.90 (dd, 1 H), 4.18 (t, 2H), 3.87 (q, 2H), 2.07 (tt, 2H).

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; N.V. ORGANON; WO2009/10491; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Continuously updated synthesis method about Methyl 4-amino-3-iodobenzoate

The chemical industry reduces the impact on the environment during synthesis Methyl 4-amino-3-iodobenzoate. I believe this compound will play a more active role in future production and life.

Application of 19718-49-1, 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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

Intermediate 4; Methyl 3-r2-alpha2-r(1.1-dimethylethyl)oxy1-2-oxoethyl)oxy)ethv?-2-(trimethylsilyl)-1H- indole-5-carboxylate FOPI/U1435/60/1; Pd(OAc)2 (106 mg, 0.47 mmol) was added to a solution of methyl 4-amino-3-iodobenzoate (2.58 g, 9.3 mmol), 1 ,1-dimethylethyl {[4-(trimethylsilyl)-3-butyn-1-yl]oxy}acetate (Intermediate 3) (3.8 g, 14.8 mmol), LiCI (394 mg, 9.3 mmol), Cs2CO3 (7.58 g, 23.25 mmol) and tri-o-tolylphosphine (143 mg, 0.47 mmol) in anhydrous DMF. The reaction mixture was stirred at 100 0C for 3 hours. The reaction mixture was filtered and rinse with dichloromethane. The filtrate was washed with brine, dried over Na2SO4, filtered and evaporated. The residue was purified on SiO2 eluting with dichloromethane to give the title compound (1.65 g, 44%). LC/MS : m/z 406 (M+H)+, Rt: 3.96.

The chemical industry reduces the impact on the environment during synthesis Methyl 4-amino-3-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2009/47240; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

The important role of C7H6BrI

The synthetic route of 116632-39-4 has been constantly updated, and we look forward to future research findings.

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. 116632-39-4, name is 5-Bromo-2-iodotoluene, A new synthetic method of this compound is introduced below., Computed Properties of C7H6BrI

0185] At -78 C, DIBAL/Hexanes (1 .0 M, 0.52 mL) was added dropwise into the solution of (2R,3S,4R,5R,6S)-3,4,5-tribenzyloxy-6- (benzyloxymethyl)tetrahydropyran-2-carbonitrile (0.258 g, 0.47 mmol) in CH2CI2 (5 mL). Then the mixture was warmed slowly to -40 C over 1 h. 0.5 N HCI aqueous was used to quench the reaction and EtOAc was used for extraction. The organic layer was collected, dried with Na2SO4 and concentrated to give (2S,3R,4S,5R,6S)-3,4,5- tribenzyloxy-6-(benzyloxymethyl)tetrahydropyran-2-carbaldehyde (0.235 g) as crude product for the next step without further purification. Into another flask containing 5- bromo-2-iodotoluene (0.42 mL, 3.0 mmol) in ether (5 mL) was added BuLi/Hexanes (2.5 M, 1 .0 mL) at -78 C. One hour later, (2S,3R,4S,5R,6S)-3,4,5-tribenzyloxy-6- (benzyloxymethyl)tetrahydropyran-2-carbaldehyde (0.235 g) was added. The mixture was warmed slowly to -20 C over 1 h 40 min. 0.5 N HCI aqueous was used to quench the reaction and EtOAc was use for extraction. The organic layer was collected, dried with Na2SO and concentrated. The resulting residue was purified by silica gel chromatography with a EtOAct Hexane gradient as eluent to give (4-bromo-2-methyl- phenyl)-[(2R,3R,4S,5R,6S)-3,4,5-tribenzyloxy-6-(benzyloxymethyl) tetrahydropyran-2- yl]methanol (A), (0.130 g) in 38% yield. MS (ESI): found [M + Na+], 745.4.

The synthetic route of 116632-39-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WASHINGTON UNIVERSITY; JANETKA, James W.; HAN, Zhenfu; HULTGREN, Scott; PINKNER, Jerry; CUSUMANO, Corinne; WO2014/194270; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Brief introduction of 444-29-1

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Formula: C7H4F3I

Example 284; (S)-1,4-Dibenzyl-2-[2-(2-trifluoromethyl-phenyl)-ethyl]-piperazine; Combine (S)-1, 4-dibenzyl-2-vinyl-piperazine (6.0 g, 20.52 mmol) and 9- borabicyclo [3.3. 1] nonane (164.1 ml, 82.07 mmol, 0.5 M in THF) and stir at ambient temperature. After 24 hrs, add 1-iodo-2-trifluoromethyl-benzene (8.37 g, 30.78 mmol), triphenylphosphine (861.0 mg, 3.28 mmol), tetrakis (triphenylphosphine) palladium (0) (474.1 mg, 0.41 mmol), and 3N NaOH (16.8 ml) and stir at 60°. After 22 hrs, remove the THF under vacuum and dissolve the residue in ethyl acetate. Wash the organic layer with 1N NaOH then combine, wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Purify the residue using ethyl acetate/hexanes (5: 95) and reduce the appropriate fractions to residue. Stir the residue in 2N NaOH, and extract with diethyl ether. Wash the organic with 1N H2SO4 then adjust the aqueous to pH 14. Extract the aqueous with diethyl ether and combine, wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Recrystallize the residue in warm ethanol to give 2.67 g (30percent) of the title compound: mass spectrum (ion spray): mp 77°-82° ; m/z = 439.2 (M+1) ; Analysis for C27H29F3N2 : calcd: C, 73.95 ; H, 6.67 ; N, 6.39 ; found: C, 74.11 ; H, 6.68 ; N, 6.50.

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2003/82877; (2003); A1;,
Iodide – Wikipedia,
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A new synthetic route of C4H8I2

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Synthetic Route of 628-21-7, 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 628-21-7 as follows.

Example 38: Synthesis of 2-(2,6-Dimethyl-phenyl)-l-oxo-octahydro-isoindole-3a- carboxylic acid (3,5-bis-trifluoromethyl-phenyl)-amide[0190] a) Lithium bis(trimethylsily)amide (1.0 M in THF, 3.8 mL, 2.4 mmol) was added to a solution of l-(2,6-dimethyl-phenyl)-5-oxo-pyrrolidine-3 -carboxylic acid methyl ester (0.4 g, 1.6 mmol) in THF (16 mL) in a reaction flask at -50 C and stirred for 5 min. The reaction was then warmed to 0 C, and addition of 1,4-diiodobutane (0.79 g, 2.6 mmol) was followed. The reaction was warmed to room temperature and stirred for 1 h. The reaction quenched saturated NH4C1. The layers were separated and the aqueous layer was extracted with EtOAc (3X). The combined organic layers were dried (MgS04) and concentrated under reduced pressure. The residue was purified by flash chromatography (Si02, 0-50% hexanes/EtOAc) to give the desired compound in 63% yield (0.3 g).

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CHEMOCENTRYX, INC.; CHARVAT, Trevor T.; CHU, Hiufung; KRASINSKI, Antoni; LANGE, Christopher W.; LELETI, Manmohan Reddy; POWERS, Jay P.; PUNNA, Sreenivas; SULLIVAN, Timothy J.; UNGASHE, Solomon; WO2011/35332; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com