Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 624-76-0, name is 2-Iodoethanol, 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 624-76-0, Formula: C2H5IO

(i) Preparation of (2-iodoethoxy)-tert-butyldimethylsilane To a stirred solution of 2-iodoethanol (17.2 g; 100 mmol) and imidazole (8.17 g; 120 mmol) in dichloromethane (100 mL) was added tert-butyldimethylsilyl chloride (15.83 g; 105 mmol) at such a rate that the reaction temperature did not rise above 30 C. Upon complete addition the solution was left stirring for 17 h, then washed with water (2*50 mL) and brine (50 mL) and dried over MgSO4. Evaporation of the solvent afforded the target compound (28.0 g; 97.8 mmol; 98%) as a colourless liquid. 1H-NMR (400 MHz) (CDCl3): delta=3.83 (t, 2H, J=7.0 Hz), 3.83 (t, 2H, J=7.0 Hz), 3.20 (t, 2H, J=7 Hz), 0.90 (s, 9H), 0.08 (s, 6H) ppm.

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:
Patent; DRIVER, Michael; TARBIT, Brian; GEHRE, Alexander; US2013/59970; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 624-75-9, 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. 624-75-9 name is 2-Iodoacetonitrile, 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: A solution of Et3B (0.5 mL, 1.0 M in EtOH, 0.5 mmol) was added over 2 h by syringe pump to a stirred mixture of the iodide 2, 4,or 5 (2.0 mmol) and olefin 1 (1 mmol) in EtOH-H2O (1:1, 10 mL) in the dark and open to air. After complete addition, the brown mixture was allowed to stir for 1 h at r.t. DBU (457 mg, 3 mmol) was added at 0 C, and the mixture was stirred at r.t. overnight. After addition of a sat. aq solution of NH4Cl (50 mL), the mixture was extracted with Et2O (20 and 10 mL), and the organic phases were washed with brine (10 mL). The combined organic layers were dried over Na2SO4 and concentrated. The crude product was purified by column chromatography.

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

Reference:
Article; Meyer, Daniel; Vin, Estelle; Wyler, Benjamin; Lapointe, Guillaume; Renaud, Philippe; Synlett; vol. 27; 5; (2016); p. 745 – 748;,
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. 624-75-9, name is 2-Iodoacetonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C2H2IN

General procedure: Individual solutions of secondary N-alpha-trimethylsilylmethyl-N-benzylamines19 (5mmol) in acetonitrile (100mL) containing K2CO3 (10mmol) and 2-iodoacetonitrile (4.5mmol) were stirred for 12hat room temperature and concentrated in vacuo to give residues that were partitioned between water and CH2Cl2. The CH2Cl2 layers were dried and concentrated in vacuo to afford residues that were subjected to silica gel column chromatography (EtOAc/hexane=1: 15 – 1: 30) to yield corresponding alpha-aminonitiriles 11a18 (91%), 11b (74%), 11c (78%), 11d (85%), 11e (75%), 11f (75%), 11g (74%), 11h (75%), 11i (78%), 11j (78%) and 11k (66%).

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:
Article; Lim, Suk Hyun; Cho, Dae Won; Choi, Jungkweon; An, Hyunjun; Shim, Jun Ho; Mariano, Patrick S.; Tetrahedron; vol. 73; 44; (2017); p. 6249 – 6261;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 7681-82-5,Some common heterocyclic compound, 7681-82-5, name is Sodium iodide, molecular formula is INa, 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 round-bottomed flask were added dichloride(pentamethylcyclopentadienyl)iridium(III) dimer (0.1 mmol, 79.5 mg) and sodium iodide (1 mmol, 150 mg). The round-bottomed flask was equipped with a reflux condenser and capped with a rubber septum. An ultrapure argon flow was passed through the system for 30 min. Then, anhydrous acetone (10 mL) was added using syringe and needle, the ultrapure argon flow was reduced, and the reaction mixture was refluxed under stirring for 3 h. Afterwards, the solvent was evaporated under reduced pressure to give a solid which was dissolved in CH2Cl2 (20 mL), washed with distilled water (3 x 10 mL), and dried over Na2SO4. After filtration, the solvent was evaporated under reduced pressure, affording the desired catalyst. Yield: 107 mg (92%); reddish solid; Rf = 0.41 (eluent: dichloromethane); 1H NMR (300 MHz, CDCl3): delta 1.76 (s, 30H); 13C NMR (75 MHz, CDCl3): delta 88.8, 10.7; IR (KBr, cm-1) 3442.9, 2918.3, 1629.9; HRMS (ESI): m/z [M – I]+ calcd for C20H30I3Ir2: 1036.8740; found: 1036.8713

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

Reference:
Article; Correa, Bianca K.; Silva, Tamiris R.C.; Raminelli, Cristiano; Tetrahedron Letters; vol. 59; 39; (2018); p. 3583 – 3585;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 624-76-0, The chemical industry reduces the impact on the environment during synthesis 624-76-0, name is 2-Iodoethanol, I believe this compound will play a more active role in future production and life.

N-methylaniline (5 mls, 0.05 mol) was reacted with 2-Iodoethanol (3.599 mls, 0.05 mol) and diisopropylethylamine (8.039 mls, 0.05 mol) in ACN at 70 C. for 16 hours. The solvent was evaporated and the residue was purified by silica gel column chromatography with hexane/EtOAc to provide the compound as a yellow orange oil, 2a (4.48 g, 0.03 mol, 64.5% yield). 1H NMR (400 MHz, Chloroform-d) delta 7.27-7.15 (m, 2H), 6.81-6.67 (m, 3H), 3.74 (t, J=5.8 Hz, 2H), 3.42 (t, J=5.8 Hz, 2H), 2.92 (s, 3H).

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

Reference:
Patent; CINCINNATI CHILDREN’S HOSPITAL MEDICAL CENTER; UNIVERSITY OF CINCINNATI; Merino, Edward J.; Mulloy, James C.; Li, Guorui; Bell-Horwath, Tiffany; US2013/230542; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 624-75-9, name is 2-Iodoacetonitrile, molecular formula is C2H2IN, 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: 2-Iodoacetonitrile

The compound obtained in Example 21 (4.6 g, 15.35 mmol) and potassium carbonate (10.6 g, 76.73 mmol) were added to acetone (100 mL) and refluxed for 2 hours by heating. To this reaction mixture was dropwise added iodoacetonitrile (1.34 mL, 18.42 mmol), and refluxed over 2 hours. The acetone was removed by vacuum distillation, and to the residue were added water (200 mL) and ethyl acetate (200 mL). The organic layer was dried over anhydrous magnesium sulfate and distillated in a vacuum. The concentrate was subjected to column chromatography (silica gel, ethyl acetate-hexane 2:3 v/v) to afford a mixture of 2:1 of [4-(2-chloropyridin-4-yl)-3-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile and [4-(2-chloropyridin-4-yl)-5-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile as yellow oil. These two regioisomers (4.78 g, 92%) were used in the next reaction step without separation.[4-(2-Chloropyridin-4-yl)-3-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile: 1H NMR (CDCl3) delta 2.29 (s, 3H), 3.71 (s, 3H), 5.19 (s, 2H), 6.73 (s, 1H), 6.75 (s, 1H), 6.85 (s, 1H), 7.06 (d, J=4.4 Hz, 1H), 7.26 (s, 1H), 7.79 (s, 1H), 8.24 (d, J=4.8 Hz, 1H); 13C NMR (CDCl3) delta 21.53, 39.97, 55.29, 110.91, 111.12, 113.65, 115.67, 118.75, 121.59, 121.65, 122.78, 130.58, 132.37, 140.16, 143.28, 149.68, 151.45, 151.79, 159.71, 162.33.[4-(2-Chloropyridin-4-yl)-5-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile: 1H NMR (CDCl3) delta 2.39 (s, 3H), 3.83 (s, 3H), 4.94 (s, 2H), 6.63 (s, 1H), 6.74 (s, 1H), 6.92-6.96 (m, 2H), 7.19 (s, 1H), 7.93 (s, 1H), 8.17 (d, J=5.2 Hz, 1H); 13C NMR (CDCl3) delta 21.56, 37.78, 55.48, 112.15, 113.91, 117.08, 118.16, 119.88, 121.36, 122.48, 128.46, 139.57, 141.60, 142.19, 142.85, 149.78, 151.95, 160.48.To a solvent mixture of THF and water (4:1, 10 mL) were added the mixture prepared in Example 22 (100 mg, 0.30 mmol), phenylboronic acid (43.9 mg, 0.36 mmol), dichlorobis(triphenylphosphine)palladium (II) (11 mg, 0.02 mmol) and potassium carbonate (42 mg, 0.30 mmol), and stirred at 70 C. for 12 hours under nitrogen atmosphere. The reaction mixture was cooled at room temperature, washed with ice water (100 mL) and extracted with ethyl acetate (100 mL×3). The organic extract was dried over anhydrous magnesium sulfate and distilled under vacuum. The residue was subjected to prep-TLC using a solvent mixture of ethyl acetate/hexane to purify the desired products.Purification yield by prep-TLC (silica gel, ethyl acetate-hexane, 1:3, v/v): (70 mg, 62%); m.p. 51-52 C.; 1H NMR (CDCl3) delta 2.41 (s, 3H), 3.81 (s, 3H), 4.95 (s, 2H), 6.76 (s, 1H), 6.82 (s, 1H), 6.95 (s, 1H), 7.06 (d, J=4.5 Hz, 1H), 7.41-7.44 (m, 3H), 7.58 (s, 1H), 7.80 (d, J=6.3 Hz, 2H), 8.01 (s, 1H), 8.53 (d, J=4.8 Hz, 1H) 13C NMR (CDCl3) delta 21.57, 37.76, 55.49, 112.31, 114.07, 116.90, 118.29, 119.60, 119.70, 122.75, 126.83, 128.71, 129.03, 129.11, 139.21, 139.61, 140.45, 141.47, 141.89, 149.88, 157.70, 160.51.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 624-75-9, its application will become more common.

Reference:
Patent; LEE, So Ha; Yoo, Kyung Ho; Oh, Chang Hyun; Han, Dong Keun; El-Deeb, Ibrahim Mustafa; Park, Byung Sun; Jung, Su Jin; US2011/15395; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 627-32-7, 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. 627-32-7, name is 3-Iodo-1-propanol belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

25 g (0.134 mol) of 3-iodopropanol, 26 g (0.202 mol) of diisopropylethylamine and 150 mL of 1,2-dichloroethane Add 250mL three-necked flask, cooled to 0 .Under stirring, a solution of 56.9 g (0.202 mol) of trifluoromethanesulfonic anhydride was slowly added dropwise at a temperature of 0 C. After the addition was completed, the temperature was naturally raised to room temperature and the reaction was allowed to proceed overnight.After the reaction was completed, 30 mL dilute hydrochloric acid (0.1 mol / L) was added to the reaction solution, and the mixture was separated by stirring to extract the organic phase. The organic phase was washed with 0.1 mol / L sodium carbonate aqueous solution and saturated sodium chloride aqueous solution, The organic phase was dried over anhydrous sodium sulfate and concentrated to give 33 g of 3-iodopropyltrifluoromethanesulfonate in a yield of 77%.

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-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hebei Sangdiya Pharmaceutical Co., Ltd.; Liu Haitao; Yang Xin; Han Yuchao; Ru Qingke; He Lei; Xia Junyi; Lang Hengyuan; (8 pag.)CN106588731; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 7681-82-5, name is Sodium iodide, 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 7681-82-5, Formula: INa

under a nitrogen atmosphere, and imidazolium salt 2d (20 mg, 0.03 mmol) was added to a 25mL Schlenk tube and dissolved in methylene chloride (2mL). Here silver oxide (7.0 mg, 0.30 mmol) was added, the dark, was stirred at room temperature for 16 hours. The nonbody precipitated afterthe reaction was removed by celite, by distilling a solution to quantitatively obtain silver (Ag) complex compound 7d of interest. Here, methylenechloride (2 mL) was added, PdCl 2 (MeCN) 2 (3.9 mg, 0.015 mmol) and the mixture was stirred at room temperature for 20 hours. After the reactionwas obtained 8d by distilling off the solvent (17.5mg). This was dissolved in methylene chloride (2 mL), sodium iodide (45 mg, 0.3 mmol) and themixture was stirred at room temperature for 20 hours. By distilling off the solvent after the reaction, to obtain a palladium (Pd) complex compound 9dof interest (yield: 19.8mg, 0.012mmol, yield: 80%).

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, Sodium iodide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; National Institute of Advanced Industrial Science and Technology; Taira, Toshiaki; Imura, Tomohiro; Komura, Nagatoshi; Kitamoto, Dai; (34 pag.)JP2016/98194; (2016); A;,
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. 624-76-0, name is 2-Iodoethanol, This compound has unique chemical properties. The synthetic route is as follows., Formula: C2H5IO

Add to the reaction bottleThioacetic acid (874 mg, 11.5 mmol),2-iodoethanol (1.72 g, 10 mmol),Dissolved in 15 ml of anhydrous toluene,1,8-diazabicycloundec-7-ene (DBU, 1.75 g, 11.5 mmol) was added dropwise at 0 C.5 ml of toluene solution, plus,The reaction was stirred for 2 hours at room temperature.After TLC detects the reaction,Dilute with a small amount of water,Divide the organic phase,Washed with saturated brine and concentrated.Purified by column chromatography,The product was dried under vacuum to give 576 mg,yield: 48%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 624-76-0.

Reference:
Patent; Shenzhen Tajirui Bio-pharmaceutical Co., Ltd.; Wang Yihan; Zhao Jiuyang; (46 pag.)CN109485676; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 7681-82-5, name is Sodium iodide, 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 7681-82-5, Recommanded Product: 7681-82-5

NaI (73 mg, 0.487 mmol) in CH2Cl2 (5 ml) was added to[Ni(Cl2(Lbenz)] 3a (90 mg, 121 mmol) in CH2Cl2 (10 ml). The mixturewas stirred 24 h, was filtered over Celite and was concentrated by volume to afford 100mg (90%) of 3c as a red solid that was isolatedby filtration. 1H NMR (CDCl3): d 7.62 (d, J 7.2, ortho, 4H, -C6H5),7.40 (t, J 7.6, meta, 4H, -C6H5), 7.31 (t, J 7.6, para, 2H, -C6H5),7.19e7.22 (m, 4H, benzimi -CH]CH), 7.13e7.15 (m, 4H, benzimi),5.29 (bs, 8H, -benzimi-NCH2), 3.75 (s, 4H, -NCH2Ph), 3.11 (bs, 8H,PhCH2CH2CH2), 2.59 (t, J 5.6, 8H, CH2NCH2Ph). 13C NMR (CD2Cl2):d 190.4, 141, 136, 129.5, 128.8, 127, 122, 109.6, 60, 54, 46, 30, 28. 13CNMR (CDCl3): d 190, 140, 136, 129, 128.7, 127, 122, 109, 59.5, 53, 46,27. HR FT-ICR MS: found 462.0680 (calcd for C40H46I2N6NiH, m/z[3c H]2 462.0686).

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; Thapa, Rajesh; Kilyanek, Stefan M.; Journal of Organometallic Chemistry; vol. 901; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com