Introduction of a new synthetic route about 4-Iodo-2-methylaniline

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 13194-68-8, A common heterocyclic compound, 13194-68-8, name is 4-Iodo-2-methylaniline, molecular formula is C7H8IN, 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.

4-iodo-2-methylbenzenamine 24 (233 mg, 1 mmol) on reaction with 1-tert-butyl-4-ethynylbenzene (25b, 158 mg, 1 mmol) by employing Sonagashira coupling conditions using Pd(PPh3)4 (69.3 mg, 0.06 equiv) as catalyst, Cul (22.8 mg, 0.12 equiv) as cocatalyst, butyl amine (261 mg, 3 equiv) as base and ether as solvent and kept the reaction for 6 h. After completion of the reaction as indicated by TLC and the reaction mixture is extracted into ether (4×25 mL) from the aqueous layer and concentrated in vacuo. The compound was further purified by column chromatography using 60-120 silica gel (ethyl acetate/hexane,1:9) to obtain 4-((4-tert-butylphenyl) ethynyl)-2-methyl benzene amine (26b) as pure product. Anthranilic acid (27, 137 mg, lmmol) on reaction with acetic anhydride at 150 C. and reflux for 30 min, after completion of reaction aqueous sodium bicarbonate solution is added and extracted in ethyl acetate (4×25 mL) from the aqueous layer and concentrated in vacuo afforded 2-methyl 4H-benzo[d][1,3]oxazin-4-one compound ( 28) as pure product. To a stirred solution of 4-((4-tertbutylphenyl)ethynyl)-2-methylbenzenamine (26b, 263 mg, 1 mmol) with 2-methyl-4H-benzo[d][1,3]oxazin-4-one (28, 161 mg, 1 mmol) in acetic acid and reflux for 8 h After completion of the reaction as indicated by TLC. then the reaction mixture was quenched with NaHCO3 and extracted in ethyl acetate (4×25 mL) from the ice cold aqueous layer and dried over anhydrous Na2SO4 afforded 3-(4-((4-tert-butylphenyl)ethynyl)-2-methylphenyl)-2-methylquinazolin-4(3H)-one (29b). Reaction of 3-(4-((4-tert-butylphenyl)ethynyl)-2-methylphenyl)-2-methylquinazolin-4(3H)-one (29b, 406 mg, 1 mmol) with 2,4-dihydroxybenzaldehyde (30d, 138 mg, 1 mmol) was taken in acetic acid Then the resulting mixture was stirred under reflux conditions for 8 h and then the reaction mixture was quenched with NaHCO3 and extracted in ethyl acetate (4×25 mL) from the ice cold aqueous layer and dried over anhydrous Na2SO4.The resulting product ( 5d) was purified by column chromatography employing EtOAc/Hexane as an eluent.

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.

The origin of a common compound about Ethyl-3-iodobenzoate

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

Electric Literature of 58313-23-8, 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. 58313-23-8 name is Ethyl-3-iodobenzoate, 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.

A dry and argon-flushed round-bottomed flask equipped with a magnetic stirring bar was charged with ethyl 3-iodobenzoate (178 mg, 0.64 mmol, 3.75 eq.) in dry THF (1.0 mL) and cooled to -20 C. A solution of isopropylmagnesium chloride-lithium chloride complex (1.3M in THF, 0.33 mL, 0.43 mmol, 2.5 eq.) was added dropwise and the resulting mixture was stirred at – 20 C for 1 h. To the reaction mixture, was then added aldehyde 5 [13] (56 mg, 0.17 mmol) as a solution in THF (0.5 mL, rinsed with an additional 0.5 mL), and the mixture was stirred at – 20 C for 25 min. The reaction was quenched by adding methanol (0.5 mL) and diluting with water (5 mL). The whole mixture was extracted with ethylacetate (20 mL x 3). The combined organic layers were washed with brine (5 mL), dried over sodium sulfate and filtered. Evaporation of the filtrate afforded a residue, from which 6a (68 mg, colorless solid, 86%) was separated by silica gel column chromatography (ethyl acetate: n-hexane 1: 15) as a C22-epimeric mixture (77:23). 6a: 1H NMR (400 MHz, TMS, CDCl3) d – 0.01 (6H x 0.23, s), 0.01 (6H x 0.77, s), 0.70 (3H, d, J 6.8 Hz), 0.88 (9H x 0.23, s), 0.90 (9H x 0.77, s), 0.95 (3H x 0.77, s), 0.96 (3H x 0.23, s), 1.40 (3H, t, J 7.1 Hz), 3.97 (1H x 0.23, s), 4.03 (1H x 0.77, m), 4.38 (2H, q, J 7.2 Hz), 4.89 (1H x 0.23, d, J 3.2 Hz), 4.98 (1H x 0.77, s), 7.41 (1H, t, J 7.7 Hz), 7.51 (1H, d, J 7.7 Hz), 7.92 (1H, d, J 7.7 Hz), 7.95 (1H x 0.77, s), 8.00 (1H x 0.23, s); HRMS (ESI) m/z calcd. for C28H46O4SiNa [MNa] 497.3058, found 497.3060.

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

Application of 1-Chloro-4-iodo-2-nitrobenzene

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 41252-95-3.

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. 41252-95-3, name is 1-Chloro-4-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 41252-95-3

A solution of 1-chloro-4-iodo-2-nitrobenzene 4(1) (5.64 g, 0.02 mol) and Na phenylsulfinate 4(2) (3.28 g, 0.02 mol) in DMF (80 ml) was stirred for 12 h at 120 C. Then, the reaction mixture was cooled, poured into water and extracted with ethyl acetate. Organic layer was dried over Na2SO4, filtered and evaporated to dryness. The mixture was separated by means of column chromatography, eluent-ethyl acetate:hexane 1:4. It gave 2.4 g (30.6%) 4-iodo-2-nitro-1-(phenylsulfonyl)benzene 4(3).

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 41252-95-3.

Analyzing the synthesis route of 1-Iodo-2-nitro-4-(trifluoromethyl)benzene

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.

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.

A new synthetic route of 3-Iodo-4,5-dimethoxybenzaldehyde

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.

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.

Introduction of a new synthetic route about 1,10-Diiododecane

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.

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.

Simple exploration of Methyl 2-amino-5-iodobenzoate

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.

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.

The origin of a common compound about 4-Iodobenzenesulfonyl chloride

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.

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.

Some tips on 1,4-Diiodobutane

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

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.

Simple exploration of 4-Iodo-1,2-dimethylbenzene

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.

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.