Author: Jessica.F

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 5876-51-7 as follows. Product Details of 5876-51-7

A suspension of 5-iodobenzo[d][1,3]dioxole (3.00 g, 12.10 mmol), ethynyltrimethylsilane (2.01 mL, 14.52 mmol), copper (_) iodide (115 mg, 0.61 mmol), bis(triphenylphosphine)palladium(II) dichloride (424 mg, 0.61 mmol), TEA (5.06 ml, 36.29 mmol) were stirred in THF (20 mL) at ambient temperature for overnight. The reaction solvent was evaporated under reduced pressure, and the residue was purified by column chromatography with hexane/ethyl acetate (10/1, v/v) to obtain the compound 40 (2.64 g, quant. yield): 1H NMR (400 MHz, CDCl3) _ 6.98 (dd, J = 8.1, 1.6 Hz, 1H), 6.89 (d, J =1.6 Hz, 1H), 6.70 (d, J = 8.0 Hz, 1H), 5.92 (s, 2H), 0.23 (s, 9H); 13C NMR (100 MHz, CDCl3) _ 148.1, 147.4, 126.8, 116.5, 111.9, 108.4, 105.1, 101.4, 92.3, 0.1.

According to the analysis of related databases, 5876-51-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; DALBY, Kevin N.; EDUPUGANTI, Ramakrishna; TALIAFERRO, Juliana; LEE, Juhyeon; (0 pag.)WO2018/160967; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 76801-93-9

Compound B was acetylated by a mixture of acetic anhydride and acetic acid (concentration about 91 v/v %, 2.0 L/kg Compound B) at 50-125C in the presence of catalytic amounts of p-toluene sulphonic acid. Excess acetic anhydride and acetic acid were distilled off under reduced pressure, and the resulting viscous solution diluted with methanol and water and hydrolysed by addition of aqueous sodium hydroxide at 50-60C to a stable pH of about 12. Hydrochloric acid (17.5 w/w %) was added to a pH of about 10.5-11.5 at 60C. Then, seeds of crystalline Compound A (0.004 kg/kg Compound B) were added, and pH was further adjusted to 6.5-7.5 by hydrochloric acid (17.5 w/w %). At this stage the solvent composition was approximately 25 % methanol and 75 % water, with a total mother liquor volume of about 3.8 L/kg Compound A. In reactor A of each experiment a certain fraction of the mother liquor volume was removed by distillation, either at atmospheric or reduced pressure (95-100C at atmospheric pressure, 55-60C under reduced pressure). In reactor B nothing was distilled off. The content of both reactors were then allowed to cool gradually to 15C over 10-12 hours before filtration, wash with methanol and drying under reduced pressure and elevated temperature. The purity of the crystals was measured by HPLC. The following results were obtained:

The synthetic route of 76801-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GE Healthcare AS; EP2281791; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 1094759-93-9,Some common heterocyclic compound, 1094759-93-9, name is 4-Chloro-5-fluoro-2-iodoaniline, molecular formula is C6H4ClFIN, 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.

To a solution of compound 12b (450 mg, 1.66 mmol) in MeOH (10 mL) and DMF (20 mL) was added Pd (OAc) 2 (38 mg, 0.17 mmol), DPPF (94 mg, 0.17 mmol) and Et 3N (504 mg, 4.98 mmol). The resulting mixture was purged and degassed with CO for 3 times, then stirred at 80C under CO (50 Psi) for 24 h. The reaction mixture was filtered and diluted with EtOAc (50 mL). The organic layer was washed with brine (50 mL), dried and concentrated under reduced pressure to give the crude residue, which was purified by column chromatography on silica gel (petroleum ether/EtOAc = 50/1 (v/v)) to give compound 12c (320 mg, 95% yield) as a white solid. LCMS: R t = 0.941 min in 5-95AB_1.5 min_220&254 chromatography (MERCK RP18 25-2mm), MS (ESI) m/z= 203.9 [M +H] +. 1H NMR (400MHz, MeOH-d 4) delta 7.83 (d, J=8.4 Hz, 1H), 6.59 (d, J=11.6 Hz, 1H), 3.85 (s, 3H).

The synthetic route of 1094759-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DIZAL (JIANGSU) PHARMACEUTICAL CO., LTD; LI, Zhengtao; ZOU, Hao; ZHU, Wei; SHEN, Changmao; WANG, Rumin; LIU, Wengeng; CHEN, Xiang; TSUI, Honchung; YANG, Zhenfan; ZHANG, Xiaolin; (307 pag.)WO2019/149164; (2019); 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. 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C8H9IO2

3-[4-(3,4-Dimethoxyphenyl)-but-3-ynyl]-1,3-oxazolidin-2-one (34). Triethylamine (0.08 mL, 0.574 mmol) and Pd(PPh3)Cl2 (8.0 mg, 0.011 mmol) were added to a mixture of 3,4-dimethoxyphenyl iodide (33) (64 mg, 0.242 mmol) and alkyne 25 (34 mg, 0.245 mmol) in THF (3 mL) at room temperature. Then Cu(I)I (5 mg, 0.026 mmol) was added. The resulting mixture was stirred at room temperature for 4 h. The reaction was quenched with water (10 mL) and concentrated to remove the organic solvents. The residue was diluted with ethyl acetate (15 mL). The organic layer was separated and washed with brine (2.x.10 mL), dried over sodium sulfate and concentrated. The residue was purified by column chromatography on silica gel (25 g), eluting with EtOAc-hexanes (10-50percent) to afford the product 34 (54 mg) as solid in 80percent yield: mp 78-79° C. 1H NMR (300 MHz, CDCl3) delta 6.95 (dd, J=2.1 Hz, J=8.4 Hz, 1H), 6.88 (d, J=1.8 Hz, 1H), 6.76 (d, J=8.4 Hz, 1H), 4.32 (t, J=7.8 Hz, 2H), 3.86 (s, 3H), 3.85 (s, 3H), 3.73 (t, J=7.8 Hz, 2H), 3.51 (t, J=6.6 Hz, 2H), 2.67 (t, J=6.6 Hz, 2H); ESIMS m/z (rel intensity) 276.05 (MH+, 94), 298.05 (MNa+, 98). Anal. (C15H17NO4) C, H, N.

According to the analysis of related databases, 5460-32-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PURDUE RESEARCH FOUNDATION; US2008/300288; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 5458-84-4, 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. 5458-84-4, name is 1-Iodo-2-methoxy-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Cooled 140 mL pyridine in a large sealable vessel to -40 2C.Bubbled in trifluoromethyl iodide from a gas cylinder, whichhad been kept in freezer overnight. After adding ICF3 for20 min, added 2-iodo-5-nitroanisole (24.63 g) and copperpowder (67.25 g). Sealed vessel and stirred vigorously for22 h at 140 2C After cooling to -50 aC, carefully unsealedreaction vessel and poured onto ice and Et20. Repeatedlywashed with Et20 and H20. Allowed the ice – Et20 mixture towarm to RT. Separated layers, washed organic layer with INHC1 (3x) , then brine, dried over Na2S04, filtered andconcentrated in vacuo. Eluted material through silica gelplug (4.5:1 Hex:CH2Cl2) to provide 5-nitro-2-trifluoromethylanisole.

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-Iodo-2-methoxy-4-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AMGEN INC.; WO2006/12374; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 31599-60-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 31599-60-7 name is 1-Iodo-2,3-dimethylbenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: To a 25mL of oven-dried Schlenk tube equipped with a magnetic stir bar was charged with [Pd(C3H5)Cl]2 (3.7mg 0.01mmol, 0.05 equiv), XPhos (10.5mg, 0.022mmol, 0.11 equiv), K2CO3 (69.1mg, 0.5mmol, 2.5 equiv), and dry CH3CN (1mL). After stirring for about 15minat r.t. under argon, a solution of aryl iodide 1 (0.24mmol, 1.2 equiv), alkylating reagent 2 (0.2mmol, 1.0 equiv), 5-Norbornene-2-carboxylic acid N4 (5.5mg, 0.04mmol, 0.2 equiv) in dry MeCN (1mL) was added, then heated to 70C and stirred for 5-24h. The reaction was monitored by TLC, after completion of the reaction, the mixture was cooled to r.t., filtered through a thin pad of celite eluting with ethyl acetate (10mL), and the combined filtrate was concentrated in vacuo. The residue was directly purified by column chromatography on silica gel or purified by PTLC to give the desired product 3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-2,3-dimethylbenzene, and friends who are interested can also refer to it.

Reference:
Article; Liu, Ze-Shui; Qian, Guangyin; Gao, Qianwen; Wang, Peng; Cheng, Hong-Gang; Hua, Yu; Zhou, Qianghui; Tetrahedron; vol. 75; 12; (2019); p. 1774 – 1780;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows.

To a solution of ethyl 2-(6-nitropyridin-3-yl)acetate (33 g, 160 mmol) in DMF (150 mL) was added NaH (13 g, 330 mmol) (60 % in oil) at 0 C. The reaction mixture was stirred for 15 min while warming to RT. After 15 min the reaction mixture was cooled to 0 C and 1,3-diiodopropane (37 mL, 330 mmol) was added. After stirring at 0 C for 30 min, the reaction mixture was warmed to RT and was stirred for 1 h. After 1 h, saturated NH4C1 (500 mL) was added, followed by the addition of water (500 mL). The reaction mixture was washed with EtOAc (500 mLx3). The combined organics were washed with brine (200 mL), dried over anhydrous Na2SC>4, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography (Petroleum ether/EtOAc =30/1 to 20/1) to afford ethyl l-(6- nitropyridin-3-yl)cyclobutanecarboxylate. MS (ESI) calc’d [M+H]+, 251; found, 251.

The chemical industry reduces the impact on the environment during synthesis 1,3-Diiodopropane(stabilized with Copper chip). I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK SHARP & DOHME CORP.; WHITE, Catherine M.; ACHAB, Abdelghani; BHARATHAN, Indu T.; FRADERA, Xavier; HAN, Yongxin; LI, Derun; LIM, Jongwon; LIU, Kun; MCGOWAN, Meredeth Ann; SCIAMMETTA, Nunzio; YU, Wensheng; ZHANG, Hongjun; ZHOU, Hua; (107 pag.)WO2019/74749; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 2142-70-3, name is 1-(2-Iodophenyl)ethanone, 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 2142-70-3, Computed Properties of C8H7IO

General procedure: Iodobenzene (0.50mmol), phenylacetylene (0.55mmol), NaOAc (1mmol), and dimethyl sulfoxide (DMSO, 8mL) were mixed. Well-dispersed Pd/Fe3O4GO (0.4mol%) in DMSO (2mL) was added to the mixture with vigorous stirring. After the reaction, the catalyst was separated from the solution by centrifugation. The product was extracted three times with dichloromethane (20mL) and dried using MgSO4.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Kim, Miran; Kang, Hyuntae; Park, Kang Hyun; Catalysis Communications; vol. 72; (2015); p. 150 – 155;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 375-80-4, 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. 375-80-4, name is 1,6-Diiodoperfluorohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

55.4 g (0.10 mol) of IC 6 F 12 I obtained in Reference Example 1 and 0.58 g (0.004 mol) of tert-butyl peroxide were added to a reactor having a capacity of 150 ml equipped with a stirrer and a thermometer. Next, VDF was added under reduced pressure until reaching 0.5 MPa, and then heating was carried out at 125 C. for 3 hours. Further, after cooling the reaction solution to 70 C., VDF was added to 0.5 MPa and heated at 125 C. for 3 hours. Further, after cooling the reaction solution to 70 C., VDF was added until it reached 0.5 MPa and heated at 125 C. for 5 hours. A total amount of 12.2 g (0.19 mol) of VDF was fed to the reactor.After cooling and discharge of the residual gas, 300 g of chloroform and 20.2 g (0.20 mol) of triethylamine were added to this product, and the reaction was carried out at 35 C. for 3 hours. 150 g of water and 25 g of a 10% hydrochloric acid aqueous solution were added to the obtained reaction solution, and the liquid separation operation was carried out to obtain an organic layer.Chloroform was distilled off from the organic layer, then distilled,17.8 g (yield 42%) of a 6E-T 2 T fraction (purity 99%) having a boiling point of 76 C. (13.33 kPa) of the following formula (12)3.6 g (yield 7%) of a 6E-1 T fraction (purity 97%) having a boiling point of 63 C. (4.00 kPa) of the following formula (13)9.8 g (yield 20%) of a 6E-T 3 TT fraction (purity 97%) having a boiling point of 74 C. (4.00 kPa) of the following formula (14) and 6 E- 0.8 g (yield 1%) of 2TT fraction (purity 98%) was obtained.The structure of the obtained fraction was confirmed by 1 H-NMR and 19 F-NMR.

The synthetic route of 1,6-Diiodoperfluorohexane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tosoh F-Tech Co., Ltd.; Kondo, Norihisa; Kono, Masahiro; (14 pag.)JP2015/81232; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 59528-27-7,Some common heterocyclic compound, 59528-27-7, name is (4-Iodophenyl)methanamine hydrochloride, molecular formula is C7H9ClIN, 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 (4-iodophenyl)methanamine hydrochloride (5.0 g, 18.55 mmol, 1.0 eq), (lS,2S)- Nl,N2- dimethylcyclohexane-l, 2-diamine (0.59 mL 3.71 mmol, 0.2 eq), Sodium ascorbate (368 mg, 1.86 mmol, 0.1 eq), Copper Iodide (530 mg, 2.78 mmol, 0.15 eq), Sodium azide (2.41 g, 37.1 mmol, 2.0 eq) , Et3N (3.11 mL, 22.26 mmol, 1.2 eq) and 2-(prop-2-yn-l-yloxy)tetrahydro- 2 /-pyran (2.6 g, 18.55 mmol, 1.0 eq) in Methanol (50 mL) and water (12 mL) were purged with Nitrogen for 5 minutes and heated to 55 C for over night. The reaction mixture was cooled to room temperature and filtered through 413 filter paper. Celite was added and the solvent was removed under reduced pressure and the residue was purified over silica gel (120 g) using dichloromethane/(methanol containing 12 % (v/v) aqueous ammonium hydroxide) as mobile phase. The concentration of (methanol containing 12 % (v/v) aqueous ammonium hydroxide) was gradually increased from 0 % to 6.25 % to afford (4-(4-(((tctrahydro-2/7-pyran-2- yljoxyjmcthyl)- 1 H- 1 ,2,3-triazol- 1 -yljphcnyljmcthanaminc (15, 3.54 g, 66%) as a white solid. LCMS m/z: [M + H]+ Calcd for C15H20N4O2 289.2; Found 289.2.

The synthetic route of 59528-27-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SIGILON THERAPEUTICS, INC.; SMITH, Devyn, McKinley; PERITT, David; VEISEH, Omid; HEIDEBRECHT, Richard; MILLER, Robert, James; (173 pag.)WO2019/195056; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com