Tag: M.W=200-300

Synthetic Route of 52548-63-7, The chemical industry reduces the impact on the environment during synthesis 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of imidazole carbaldehyde (1a-d) (100 mg, 1 equiv) in methanol (3 mL) were added successively Na2SO4 (0.2 g), amine 2a-d (1.2 equiv), alkynoic acid 3a-c (1.2 equiv) and isonitrile 4a-c (1.2 equiv) in a screw capped vial equipped with a magnetic stir bar. The reaction mixture was stirred at room temperature for 24-48 h in closed vial. After completion of the reaction, the mixture was diluted with dichloromethane (100 mL) and was extracted with water (50 mL). Organic layer was washed with brine (50 mL), dried over magnesium sulfate and evaporated under reduced pressure to obtained residue which was subjected to silica gel column chromatography (1-5 % methanol in dichloromethane) to afford the desired product 5a-r as 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, 5-Fluoro-2-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Zhenghua; Legras, Laetitia; Kumar, Amit; Vachhani, Dipak D.; Sharma, Sunil K.; Parmar, Virinder S.; Van Der Eycken, Erik V.; Tetrahedron Letters; vol. 55; 13; (2014); p. 2070 – 2074;,
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 35944-64-0 as follows. SDS of cas: 35944-64-0

To a suspension, previously degazed with nitrogen bubbling for 1 h, of Intermediate Gen-2-b (300 g, 1.29 mol, 1 eq.), Intermediate Gen-9-a (343.2 g, 1.35 mol, 1.05 eq.) and potassium acetate (380 g, 3.9 mol, 3 eq.) in DMSO (2.65 L), previously degazed with nitrogen bubbling for 2 h, is added PdCl2(dppf).DCM (52 g, 0.06 mol, 0.05 eq.). The reaction mixture is stirred at 80 C. under nitrogen overnight. The reaction is cooled to room temperature, then water (1.5 L) and EtOAc (3 L) are added. The biphasic solution is filtered through a plug of celite, and the cake is washed with EtOAc (2 L). The two layers of the filtrate are separated, the aqueous layer is extracted again with EtOAc (3 L) and the combined organic layers are washed with water (500 mL). The organic layer is dried over Na2SO4, filtered and evaporated to dryness. The residue is purified by chromatography on silica (elution cyclohexane/EtOAc: 95/5 to 70/30) to afford Intermediate Gen-3-a. 1H NMR (300 MHz, CDCl3-d) delta ppm 7.17 (1H, d), 6.99 (1H, d), 6.70 (1H, dd), 3.54 (2H, bs), 2.25 (3H, s), 1.36 (12H, s)

According to the analysis of related databases, 35944-64-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SANIERE, Laurent Raymond Maurice; HUCK, Jacques; DYKES, Graeme James; SCHMITT, Benoit Antoine; BLANC, Javier; BUTLER, Anna Sara; BONNATERRE, Florence Marie-Emilie; BEAUMONT, Stephane Nicolas Alain; US2015/80391; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, 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 5876-51-7, SDS of cas: 5876-51-7

[00341] In a reaction tube under nitrogen, a mixture of PdCl2(dppf)CH2Cl2 (22 mg; 0.027 mmol) and triethylamine (0.36 ml; 2.58 mmol) in dioxane (4 ml; dried over 4 ? sieves) was sealed and stirred at 80 C. overnight (18 h). After cooling to room temperature, HB(pin) (0.18 ml; 1.24 mmol), 1-iodo-3,4-methylenedioxybenzene (216 mg; 0.871 mmol) and N-methylacetamide (39 mg; 0.56 mmol) were added and the reaction mixture was stirred at 80 C. GC analysis after 30 minutes showed a new peak at 11.1 minutes (51%) which was identified by GC/MS as the desired arylborate 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, 5-Iodobenzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, 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 82998-57-0, Computed Properties of C8H7IO2

3-Iodo-4-methylbenzoic acid (1.28 g, 4.88 mmol) was suspended in DCM (25 mL). Oxalyl chloride (420 muL, 4.9 mmol) was added, followed by DMF (1 drop). The reaction was stirred at 22 C., and gas evolution was observed for around 60 minutes, at which point HPLC analysis indicated almost complete consumption of the starting material. The solvent was removed under vacuum to provide 1.38 g (101% yield) of orange oil that solidified on storage. This material was used in the next step without further purification or characterization.

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; Promega Corporation; Levin, Sergiy; Ohana, Rachel Friedman; Kirkland, Thomas; Wood, Keith V.; (117 pag.)US2016/355523; (2016); A1;,
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. 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 2-Fluoro-5-iodobenzonitrile

To a solution of Tributyl-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-2,5-dihydro-furan-3-yl]-stannane (300 mg) in N,N-dimethylformamide (12 mL) under argon was successively added 2-Fluoro-5-iodo-benzonitrile (630 mg), copper iodide (20 mg) and then tetrakis(triphenylphosphine) palladium (42 mg). The reaction was heated at 100 C under argon for 20 hours. The reaction was allowed to cool down to room temperature then water was added and the mixture was extracted with ethyl acetate. The organic extract was washed with water, dried over sodium sulfate and concentrated in vacuo to give a residue which was purified by chromatography on silica gel (eluent: heptanesdichloromethane, 2:1) to give 5-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-2,5-dihydro-furan-3-yl]-2-fluoro-benzonitrile (182 mg) as a brown solid.1H-NMR (CDCl3, 400 MHz): 7.65-7.63 (m, 2H), 7.47 (m, 2H), 7.40 (m, 1H), 7.29 (m, 1H), 6.40 (bs, 1H), 5.30 (dd, J=2.2 and 12.8 Hz, 1H), 5.17 (m, 1H) ppm. 19F-NMR (CDCl3, 376 MHz): -78.11 and -104.17 ppm.

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; SYNGENTA CROP PROTECTION LLC; US2012/329769; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 21304-38-1, 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 21304-38-1 as follows.

Step l : 2-(2′-Fluorobiphenyl-4-yl)-6-iodo- 1 H-benzimidazole Into a 10 mL pressure tube equipped with a magnetic stirbar was added 4- iodobenzene-l,2-diamine (600 mg, 2.56 mmol), 2′-fluorobiphenyl-4-carbaldehyde (513 mg, 2.56 mmol) and DMF (4 mL). The reaction mixture was treated with drop wise addition of TMSCl (0.81 mL, 6.41 mmol), the vial sealed, and the mixture heated to 90 0C for 4 h. The cooled reaction mixture was poured into a 125 mL separatory funnel containing 2 M aqueous Na2CO3 solution (75 mL) and the mixture extracted with ethyl acetate (3 x 30 mL). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. Purification by column chromatography through silica gel, eluting with 5% acetone in toluene afforded the desired product as a solid.

According to the analysis of related databases, 21304-38-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK FROSST CANADA LTD.; WO2009/129625; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 101066-87-9, name is 4-Iodo-2-(trifluoromethyl)benzonitrile, 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 101066-87-9, SDS of cas: 101066-87-9

. Step D. tert-butyl 3-(4-cvano-3-(trifluoromethyl)phenyl)pyrrolidine-l-carboxylate A suspension of tert-butyl 4-(4-cyano-3-(trifluoromethyl)phenyl)-2,3-dihydro-lH-pyrrole- 1-carboxylate and tert-butyl 3-(4-cyano-3-(trifluoromethyl)phenyl)-2,5-dihydro-lH- pyrrole-l-carboxylate (370 mg, 1.10 mmol) and Pd/C (100 mg) in THF (8 mL) was stirred under hydrogen at room temperature for 2 hours. The reaction mixture was filtered and the filtrate was concentrated to afford tert-butyl 3-(4-cyano-3- (trifluoromethyl)phenyl)pyrrolidine-l-carboxylate as a white powder (350 mg, 94%), which was used for the next step without further purification. LCMS (ESI) m/z: 285.1 [M- 56+H]+.

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; BEAUFOUR-IPSEN (TIANJIN) PHARMACEUTICAL CO., LTD.; AUVIN, Serge; LANCO, Christophe; DUTRUEL, Oliver; CHAO, Qi; GU, Kaichun; WO2015/100617; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 108078-14-4,Some common heterocyclic compound, 108078-14-4, name is 2-Iodo-3-methylbenzoic acid, 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.

Thionyl chloride [5 mL] was added to 2-iodo-3-methyl-benzoic acid (2.00 g, 7.63 mmol) at room temperature and heated to 50oC for 1 hour. The solution was then cooled and evaporated. The crude residue was dissolved in ethyl acetate, washed with brine and dried with magnesium sulfate. The crude product was then dissolved in THF [5 mL] and a 1M solution of lithium aluminum hydride [10.7 mL] was added at room temperature and stirred for 1 hour. Water [0.1 mL] and 15% NAOH [0.1 mL] were added followed by evaporation. Column chromatography (50% EtOAc in hexanes) of the residue yielded the title compound (0.50 g, 26 %) as a SOLID. 1H-NMR (CDCL3) : delta 3.20 (t, 2H, J=7. 6 Hz), 2.98 (s, 3H), 2.52 (t, 2H, J=7.2 Hz), 2.09 (m, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-3-methylbenzoic acid, its application will become more common.

Reference:
Patent; 3-DIMENSIONAL PHARMACEUTICALS, INC.; WO2003/99805; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 216393-67-8, A common heterocyclic compound, 216393-67-8, name is 4-Chloro-2-fluoro-6-iodoaniline, molecular formula is C6H4ClFIN, 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.

To a mixture of 3-ethynylpyridine (1.13 g, 11 mmol) and 2-fluoro^-chloro-6-iodoaniline (2.71 g, 10 mmol) in triethylamine (100 mL) is added PdCI2(PPh3)2 (175 mg, 0.25 mmol) and CuI (95 mg, 0.50 mmol) and the mixture is refluxed for 1 h. The solvent is removed in vacuo and the residue is purified by silica gel flash chromatography (dichloromethane- methanol, 1 :0 to 24:1 ) to give 4-chloro-2-fluoro-6-pyridin-3-ylethynyl-phenylamine. MS (ESI) m/z 247 (M+H)+.

The synthetic route of 216393-67-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; WO2009/156462; (2009); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 58313-23-8,Some common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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 -45 C. solution of ethyl 3-iodobenzoate (2.434 g, 8.8 mmol) in 40 mL THF was treated with i-PrMgCl (4.8 mL, 9.6 mmol, 2 M/ether). After 1 h, allyl bromide (1.6 mL, 18.9 mmol) was added followed by CuCN (79 mg, 0.88 mmol). The reaction was stirred for 1 h and then was quenched by addition of 50 mL saturated NH4Cl solution. Water (30 mL) was added and the resulting mixture was extracted with ethyl acetate (3*50 mL). The combined ethyl acetate solution was dried (MgSO4), filtered and evaporated. Purification by flash chromatography on silica gel (5% ethyl acetate/hexanes?10%) gave compound 7 (1.145 g, 68%).

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALLERGAN, INC.; US2009/239869; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com