Month: April 2021

Some common heterocyclic compound, 400-97-5, name is 1-Iodo-2-nitro-4-(trifluoromethyl)benzene, molecular formula is C7H3F3INO2, 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. SDS of cas: 400-97-5

To a solution of compound 52 (850 mg, 2.68 mmol) in HOAc- EtOH (10 mL, 1 :5, v/v) was added iron dust (750 mg, 13.43 mmol) at 23 C. The resulting mixture was stirred at 23 C for 3 h before it was quenched with a saturated solution of NaHC03 (20 mL) and diluted with EtOAc (50 mL). The layers were separated, and the organic layer was extracted with H20 (3 x 10 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexanes: EtOAc 10: 1 ) to give compound 53 (754 mg, 98%) as a yellow solid. (0468) [00359] 1 H NMR (400 MHz, CDCI3) delta = 7.76 (dd, J = 8.2, 0.7 Hz, 1 H), 6.96 (d, J = 1 .7 Hz, 1 H), 6.72 (ddd, J = 8.2, 2.0, 0.6 Hz, 1 H), 4.32 (brs, 2H). m/z (ESI) 288.0 [M+H+].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 400-97-5, its application will become more common.

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 32024-15-0 as follows. Recommanded Product: 3-Iodo-4,5-dimethoxybenzaldehyde

13ax) A mixture of 5.0 g of 3-iodo-4,5-dimethoxy-benzaldehyde, 1.18 g of hydroxylamine hydrochloride, 1.37 g of pyridine and 17 ml of toluene is held at reflux for 2 hrs. (see A. Saednya, Synthesis 1982, 190). The precipitate which separates after cooling is filtered off under suction. Chromatography on silica gel with methylene chloride/methanol 9:1 yields 3.09 g of 3-iodo-4,5-dimethoxy-benzonitrile as a colourless solid. Yield: 63%. Mass spectrum: peaks inter alia at m/e: 289 (100%), 274 (38%), 132 (30%), 119 (43%).

According to the analysis of related databases, 32024-15-0, the application of this compound in the production field has become more and more popular.

Reference of 16355-92-3, The chemical industry reduces the impact on the environment during synthesis 16355-92-3, name is 1,10-Diiododecane, I believe this compound will play a more active role in future production and life.

Example 1 Preparation of 2,2′-(1,12-dodecanediyl)bispyridine LDA (2M) (20 mL, 40.00 mmol) was added dropwise to a solution of 2-picoline (3.73 g, 40.00 mmol) in THF (60 mL) at -78 C. The mixture was stirred for 30 min and then 1,10-diiododecane (6.31 g, 16.00 mmol) in THF (10 mL) was added dropwise. The resulting mixture was warmed to room temperature and stirred for 4 hrs. 50% saturated NH4Cl was added to the reaction mixture. The aqueous phase was extracted with ethylacetate (40 mL*2), and the combined organic liquors were washed with 50% saturated brine (40 mL*3) and saturated brine (40 mL), dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product was purified by column chromatography (hexanes:ethylacetate 2:1 to 1:1) to afford 3.75 g of the title compound. Yield: 72%. 1H NMR (300 MHz, CDCl3) delta 1.13-1.42 (m, 16H), 1.60-1.81 (m, 4H), 2.78 (t, J=7.8 Hz, 4H), 7.08 (ddd, J=7.5, 5.1, 0.6 Hz, 2H), 7.13 (d, J=7.5 Hz, 2H), 7.57 (dt, J=7.5, 1.8 Hz, 2H), 8.52 (dd, J=5.1, 0.6 Hz, 2H) ppm; 13C NMR (75 MHz, CDCl3) delta 29.7, 29.75, 29.8, 29.9, 30.2, 38.7, 120.9, 122.8, 136.3, 149.2, 162.5 ppm.

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, 1,10-Diiododecane, other downstream synthetic routes, hurry up and to see.

Application of 77317-55-6, 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. 77317-55-6, name is Methyl 2-amino-5-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

b) (2-Amino-5-iodo-phenyl)-methanol; Intermediate 17a (14.00 g) was dissolved in dry THF (50 ml_) and 1M diisobutylaluminium hydride in THF (165 ml_) was added dropwise to this solution at -30C. The solution was then stirred at -150C for 1 h. To this mixture MeOH (50 mL) was added portionwise maintaining the temperature of the solution below -5C. The resulting mixture was then at -15C for 18 h. The formed solid was filtered off and washed with MeOH. The organic phase was dried and the solvent was evaporated in vacuo. The residue was purified by flash chromatography (silica gel, 1-5% methanol in dichloromethane) to give the title compound (9.70 g); ESMS m/z 249.9 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis Methyl 2-amino-5-iodobenzoate. I believe this compound will play a more active role in future production and life.

Electric Literature of 98-61-3, 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. 98-61-3 name is 4-Iodobenzenesulfonyl chloride, 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 25-mL oven-dried Schlenk tube, arenesulfonyl chloride (1.5-2 mmol), furan derivative (1 mmol), Li2CO3 (0.222 g, 3 mmol), 1,4-dioxane (2 mL) and PdCl2(MeCN)2 (12.9 mg, 0.05 mmol) were added successively. The mixture was evacuated by vacuum-argon cycles (5 ×) and stirred at 140 C (oil bath temperature) for 20-72 h (see tables and schemes). After cooling the reaction at r.t. and concentration, the crude mixture was purified by column chromatography (silica gel) to afford the C5-arylated furans.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Iodobenzenesulfonyl chloride, and friends who are interested can also refer to it.

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. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 1,4-Diiodobutane

1) Weigh 7.1g of pyrrolidine and 14g of potassium carbonate dissolved in acetone 1000mL, added to the three bottles, the temperature adjusted to 15 C after the slow drop1,4-diiodobutane, 13.4 mL,The whole drop reaction temperature was maintained at 15 C to 20 C,After the completion of heating to 35 C , continue to respond 24h,After the reaction is completed, the reaction solution is directly filtered,The organic solvent was distilled under reduced pressure to give 24.5 g1- (4-iodobutane) pyrrole,The yield (in terms of pyrrolidine) was 97%.

The synthetic route of 628-21-7 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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H9I

General procedure: PdCl2(PPh3)2 (0.1 mmol), P(o-tolyl)3 (0.1 mmol), TFben(0.5 mmol) and indole (1.0 mmol) were transferred into an ovendriedtube (15 mL), which was evacuated and backfilled withN2(5x). DMSO (2 mL), aryl iodide (1.2 mmol), Et3N (1 mmol) andHCO2H (1.5 mmol) were added into the tube via syringe. The reactionmixture was stirred at 70 C for 24 h. After the reaction wascomplete, the mixture was filtrated and extracted with DCM. Thecombined organic layers were washed with H2O and brine, driedover anhydrous Na2SO4, and then concentrated under vacuum.The crude product was purified by column chromatography on silicagel (petroleum ether/ethyl acetate = 20/1) to afford the product.

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.

Related Products of 2043-57-4, 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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The starting 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl iodide (12.69 g, 26.8 mmol) was dissolved in the mixture of pentane and diethyl ether (90 and 60 mL). The solution was stirred and cooled to -78 C before the solution of 1.6 M tert-butyllithium in hexane (18.54 mL, 29.7 mmol) was added. The mixture was stirred for 15 min and freshly distilled (2-chloroethyl)trichlorosilane (1.5 g, 7.58 mmol) slowly added with stirring. The reaction mixture was stirred for 2 h at -78 C and 1 h at 0 C then it was poured on ice (ca 10 g) and stirred for further 15 min. The resulting biphasic mixture was filtered through silica gel. The layers were separated and aqueous phase was extracted with diethyl ether (3×50 mL). The combined organic phases were dried (MgSO4) and evaporated to afford the product as a yellow oil. The yield was 8.1 g (7.15 mmol, 94%). 1H NMR: delta (ppm) 1.00 (m, 6H, CH2CH2CF2); 1.40 (t, 3JHH=7.7Hz, 2H, CH2CH2Cl); 2.11 (m, 6H, CH2CF2); 3.72 (t, 3JHH=7.7Hz, 2H, CH2Cl). 13C{1H} NMR: delta (ppm) 1.65 (s, CH2CH2CF2); 16.88 (s, CH2CH2Cl); 25.46 (t, 2JCF=24.0Hz, CH2CF2); 40.68 (s, CH2Cl); 106-122 (m, CF3, CF2). 19F NMR: delta (ppm) -127.05 (m, 2F, CF2); -124.09 (bs, 2F, CF2); -123.69 (bs, 2F, CF2); -122.70 (bs, 2F, CF2); -116.94 (m, 2F, CF2); -81.78 (t, 3JFF=11.1Hz, 3F, CF3). 29Si{1H} NMR: delta (ppm) 6.36 (s, 1Si).

The synthetic route of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 19821-80-8, name is 1,3-Dibromo-2-iodobenzene, 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 19821-80-8, Safety of 1,3-Dibromo-2-iodobenzene

Example 2: 2,2′,6,6′-Tetrabromo-l,l’-biphenyI (III); At -75 C butyllithium (14 mmol) in hexanes (5.6 mL) was added to a solution ofl,3-dibromo-2-iodobenzene (4.3 g, 12 mmol) in diethyl ether (0.18 L). After the solutionwas stirred for 2 h at -75 C, copper(II)chloride (9.7 g, 72 mmol) was added, and thereaction mixture was allowed to attain 25 C over a 12 h period. Cold water was added tothe reaction mixture and the organic layer was separated. The aqueous phase was extractedwith ethyl acetate (2×0.10 L). The combined organic layers were dried over sodium sulfatebefore being evaporated. 2,2′,6,6′-tetrabromo-l,l’-biphenyl precipitates upon treatment ofthe residue with hexanes cooled to -20 C. The product (9.0 g, 33%) is pure enough forfurther reaction;m.p. 214-215 C;.H NMR (CDC13, 400 MHz): 8 = 7.67 (d, J- 8.3 Hz, 4 H), 7.17 (t, J- 8.0 Hz, 2 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.

Adding a certain compound to certain chemical reactions, such as: 696-41-3, name is 3-Iodobenzaldehyde, 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 696-41-3, SDS of cas: 696-41-3

General procedure: Benzaldehyde (1.0 mmol), TMTD (1.1 mmol), CuI (10 mol%), and DTBP (4.0 equiv) were added to a dried sealed tube equipped with a septum and magnetic stirrer bar, EtOAc (2 mL) was then added. (Caution. The sealed tube is a pressure-proof tube with a septum.) The mixture was stirred at 120 C and checked by thin-layer chromatography (TLC) until the starting material was consumed (ca. 7-8 h). The reaction was cooled to r.t., quenched with sat. NH4Cl solution (5 mL), and then extracted with EtOAc (3 × 10 mL). The crude solution was dried over anhydrous Na2SO4 and evaporated under vacuum. The residue was purified by flash column chromatography to afford the desired product.

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.