Category: 124700-41-0

Electric Literature of 124700-41-0,Some common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

Intermediate 1C: (3,4-Dihydroisoquinolin-2(lH)-yl)(2-fluoro-5-iodophenyl)methanone[00165] To a suspension of 2-fluoro-5-iodobenzoic acid (Aldrich, 5.27 g, 19.8 mmol) in CH2CI2 (35.0 mL) was added oxalyl chloride (14.9 mL, 29.7 mmol, 1M solution in CH2CI2) followed by 2 drops of DMF via syringe. Gas evolution was initiated and the resulting mixture was stirred at room temperature for 2 h. The reaction mixture was then quenched with sat. aq. NH4CI solution and extracted with EtOAc (3 x). The combined organic extracts were dried over Na2S04, filtered and concentrated in vacuo to give crude 2-fluoro-5-iodobenzoyl chloride which was used directly in the next step.[00166] The crude product obtained above was dissolved in CH2CI2 (49.6 mL) and cooled to 0 C. To the solution were added 1,2,3,4-tetrahydroisoquinoline (2.7 mL, 21.8 mmol) followed by 2,6-lutidine (4.6 mL, 39.7 mmol). The resulting reaction mixture was stirred at room temperature for 1 h. The reaction mixture was washed IN HC1 (2 x) and the organic layer was extracted with CH2CI2 (2 x). The combined organic extracts were washed with sat. aq. NaCl solution and dried over a2S04. Filtration and concentration in vacuo provided the title compound (7.55 g, 95%) as a viscous, yellow oil. XH NMR (CDCI3, 1.5: 1 mixture of amide rotamers) delta 7.78-7.66 (m, 2H), 7.26-7.12 (m, 3.5H), 6.98- 6.86 (m, 1.5H), 4.92 (s, 1.5H), 4.50 (br s, 0.5H), 3.65-3.52 (m, 1.5H), 3.04-2.95 (m, 1H), 2.92-2.82 (m, 1.5H); MS(ESI+) m/z 382.1 (M+H)+.

The synthetic route of 124700-41-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BORZILLERI, Robert M.; CAI, Zhen-wei; TEBBEN, Andrew J.; PEREZ, Heidi L.; ZHANG, Liping; SCHROEDER, Gretchen M.; WEI, Donna D.; WO2012/162365; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 124700-41-0, 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. 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-Fluoro-5-iodobenzoic acid (6.60 g, 24.81 mmol) was dissolved in chloroform (70 ml) and oxalyl chloride (4.30 ml, 49.29 mmol) and dimethylformamide (catalytic amount) were added. The mixture was stirred at room temperature for 3 hrs. The reaction solution was concentrated under reduced pressure and chloroform (35 ml), was added to dissolve the residue. The obtained solution was added dropwise to a solution of ethyl 3,3-dimethylaminoacrylate (4.26 g, 29.75 mmol) and triethylamine (5.19 ml, 37.24 mmol) in chloroform (35 ml), and the mixture was stirred at room temperature for 15 hrs. Water was added to partition the reaction solution, and the organic layer was washed with saturated brine and dried over sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure and the obtained residue was purified by silica gel chromatography (ethyl acetate_hexane=1:2 to 1:1) to give an object product (6.40 g, yield 66%) of a mixture of E form and Z form as an orange solid.1H NMR(CDCl3 400MHz) (delta) ppm: 0.94 (3H, t, J=7.2Hz), 2.88 (3H, brs), 3.31 (3H, brs), 3.97 (2H, q), 6.78 (1H, dd, J=8.4, 10.0Hz), 7.65-7.67 (1H, m), 7.78(1H, s), 7,85 (1H, brs) MS (ESI) : M+ 392

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

Reference:
Patent; Japan Tobacco Inc.; EP1564210; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 124700-41-0, 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. 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The eighth compound (10.000 g, 37.592 mmol) was dissolved in 40 mL of dichloromethane and 1 mL of DMF, and stirred at room temperature. The oxalyl chloride (3.800 mL, 45.110 mmol) was dissolved in 10 mL of dichloromethane and added dropwise to the reaction system, and stirred at room temperature for 1 h. After the reaction is completed, the reaction solution is sparged.It was replaced with anhydrous toluene three times to obtain an oily liquid ninth compound.

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, 2-Fluoro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Institute of Technology; Liang Jianhua; Ma Congxuan; (36 pag.)CN109942653; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 124700-41-0, These common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-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.

2-Fluoro-5-iodobenzoyl chloride (45f) A suspension of the acid (5.37 g, 20.19 mmol) in SOCl2 (40.82 g, 25 mL, 343 mmol) was refluxed for 22h. The solvents were removed by rotary evaporation and the residue partitioned between EtOAc and saturated aqueous Na2CO3. The organic extracts were dried over MgSO4 and concentrated yielding 45f (5.36 g, 93%) as a pale pink solid which was used in the next step without further purification: 1H NMR (CDCl3) 6.96 (t, J=6.0 Hz, 1H), 7.90-7.94 (m, 1H), 8.35 (d, J=3.0 Hz, 1H).

Statistics shows that 2-Fluoro-5-iodobenzoic acid is playing an increasingly important role. we look forward to future research findings about 124700-41-0.

Reference:
Patent; PFIZER INC; US2005/90529; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 124700-41-0,Some common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

Intermediate 1C: (3,4-Dihydroisoquinolin-2(lH)-yl)(2-fluoro-5-iodophenyl)methanone[00165] To a suspension of 2-fluoro-5-iodobenzoic acid (Aldrich, 5.27 g, 19.8 mmol) in CH2CI2 (35.0 mL) was added oxalyl chloride (14.9 mL, 29.7 mmol, 1M solution in CH2CI2) followed by 2 drops of DMF via syringe. Gas evolution was initiated and the resulting mixture was stirred at room temperature for 2 h. The reaction mixture was then quenched with sat. aq. NH4CI solution and extracted with EtOAc (3 x). The combined organic extracts were dried over Na2S04, filtered and concentrated in vacuo to give crude 2-fluoro-5-iodobenzoyl chloride which was used directly in the next step.[00166] The crude product obtained above was dissolved in CH2CI2 (49.6 mL) and cooled to 0 C. To the solution were added 1,2,3,4-tetrahydroisoquinoline (2.7 mL, 21.8 mmol) followed by 2,6-lutidine (4.6 mL, 39.7 mmol). The resulting reaction mixture was stirred at room temperature for 1 h. The reaction mixture was washed IN HC1 (2 x) and the organic layer was extracted with CH2CI2 (2 x). The combined organic extracts were washed with sat. aq. NaCl solution and dried over a2S04. Filtration and concentration in vacuo provided the title compound (7.55 g, 95%) as a viscous, yellow oil. XH NMR (CDCI3, 1.5: 1 mixture of amide rotamers) delta 7.78-7.66 (m, 2H), 7.26-7.12 (m, 3.5H), 6.98- 6.86 (m, 1.5H), 4.92 (s, 1.5H), 4.50 (br s, 0.5H), 3.65-3.52 (m, 1.5H), 3.04-2.95 (m, 1H), 2.92-2.82 (m, 1.5H); MS(ESI+) m/z 382.1 (M+H)+.

The synthetic route of 124700-41-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BORZILLERI, Robert M.; CAI, Zhen-wei; TEBBEN, Andrew J.; PEREZ, Heidi L.; ZHANG, Liping; SCHROEDER, Gretchen M.; WEI, Donna D.; WO2012/162365; (2012); A1;,
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 124700-41-0 as follows. COA of Formula: C7H4FIO2

General procedure: A mixture of various carboxylic acids (1.0mmol), an excess of thionyl chrolide (5mL) was refluxed for 2h and concentrated in vacuo to give corresponding acyl chloride (quant).

According to the analysis of related databases, 124700-41-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Chen, Yin-Bo; Li, Ji-Ling; Shao, Xu-Sheng; Xu, Xiao-Yong; Li, Zhong; Chinese Chemical Letters; vol. 24; 8; (2013); p. 673 – 676;,
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 124700-41-0 as follows. COA of Formula: C7H4FIO2

General procedure: A mixture of various carboxylic acids (1.0mmol), an excess of thionyl chrolide (5mL) was refluxed for 2h and concentrated in vacuo to give corresponding acyl chloride (quant).

According to the analysis of related databases, 124700-41-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Chen, Yin-Bo; Li, Ji-Ling; Shao, Xu-Sheng; Xu, Xiao-Yong; Li, Zhong; Chinese Chemical Letters; vol. 24; 8; (2013); p. 673 – 676;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 124700-41-0, The chemical industry reduces the impact on the environment during synthesis 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

2-Fluoro-5-iodobenzoic acid (10.000 g, 37.592 mmol) was dissolved in 40 mL of dichloromethane and 1 mL of N,N-dimethylformamide, and stirred at room temperature to dissolve oxalyl chloride (3.800 mL, 45.110 mmol) 10 mL of dichloromethane was added dropwise to the reaction system, and the mixture was stirred at room temperature for 1 hour. After the reaction was completed, the reaction solution was spun dry and replaced with anhydrous toluene three times to obtain an oily liquid thirteenth Compound.

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, 2-Fluoro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Institute of Technology; Liang Jianhua; Ma Congxuan; (37 pag.)CN109942654; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 124700-41-0, These common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-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.

Preparation 29 Ethyl 3-(2-fluoro-5-iodophenyl)-3-oxopropanoate To a stirred solution of 5.32 g of 2-fluoro-5-iodobenzoic acid from Preparation No. 28 in 20 mL of THF, under argon, is added 3.9 g of carbonyldiimidazole. In a separate flask, 2.8 mL of chlorotrimethylsilane is added to a mixture of 3.74 g of potassium ethyl malonate in 20 mL of acetonitrile. The mixture is stirred under argon for 18 h, then cooled to 0 C. for the dropwise addition of 6.6 mL of DBU. The mixture is stirred for 3 h at 0 C., then the solution of acyl imidazolide prepared above is added via cannula. After 2 h, the mixture is partitioned between ether and excess dilute HCl, and the organic phase is washed with dilute HCl and brine and dried (MgSO4). Removal of the solvent under reduced pressure left a colorless oil, which is flash chromatographed on silica using 10% ethyl acetate in hexane to provide 5.07 g of the title compound as dense pinkish prisms. Physical properties as follows: 1H NMR (CDCl3) delta1.34, 4.27, 5.82, 6.89, 7.7, 8.2 ppm; IR 1624, 1485, 1419, 1245, 1193, 1070, 1028, 813 cm-1.

Statistics shows that 2-Fluoro-5-iodobenzoic acid is playing an increasingly important role. we look forward to future research findings about 124700-41-0.

Reference:
Patent; Pharmacia & Upjohn Company; US6248739; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 124700-41-0,Some common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

Compound 1 (20.0 g, 75.2 mmol, 1 eq) was dissolved in 70 mL of EtOH.Then gradually add H2SO4 (7.37g, 75.1mmol, 4.01mL, 1eq).The mixture was stirred at 100 C for 5 h.And use TLC (Dichloromethane/Methanol=10/1, Rf=0.87) The progress of the reaction was detected.When the reaction is complete,The reactants were concentrated under reduced pressure.The concentrated product was extracted (EOtOH 200 mL, NaHCO 3 saturated solution (100.0 mL x 2), and then the organic layer was taken.It was dried by adding anhydrous Na2SO4.After further evaporation to dryness the title product 2 (21.0 g, 71.4 mmol, 94.9% yield).Figure 3 shows the results of TLC chromatography for this reaction.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Fluoro-5-iodobenzoic acid, its application will become more common.

Reference:
Patent; Shanghai Health Medical School; Tang Dewei; Huang Gang; Huang Chen; Wu Xingyu; Yu Meicen; Li Yanjiao; (18 pag.)CN109942582; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com