Author: Jessica.F

Application of 460-37-7, A common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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.

Method A: 1.8 g (7.13 mmol) of the compound from Ex. 49A and 3.49 g (10.7 mmol) of caesium carbonate were stirred in 15 ml of DMF at RT for 10 min, before 1.3 ml (10.7 mmol) of 1,1,1-trifluoro-3-iodopropane were added. Subsequently, the reaction mixture was stirred at a temperature of 100 C. in a microwave oven (Biotage Initiator with dynamic control of irradiation power). After 2 h, a further 167 mul (1.43 mmol) of 1,1,1-trifluoro-3-iodopropane were added and the heating was continued for 30 min. After cooling to RT, the mixture was diluted with about 75 ml of ethyl acetate and washed successively with water and saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was evaporated to dryness. The crude product was purified by MPLC (Biotage cartridge, 100 g of SNAP KP-Sil silica gel, eluent: cyclohexane/ethyl acetate 1:2). After concentration and drying, a mixture of N- and O-alkylated product was obtained, from which it was possible to obtain the N-alkylated main product in solid form by stirring with a mixture of 30 ml of pentane and 2 ml of dichloromethane. Further N-alkylated product was obtained from the concentrated mother liquor from the stirring by means of preparative HPLC (Method 8). After concentration of the product fractions and drying under high vacuum, together with the solids from the stirring, 1.86 g (74% of theory) of the title compound were obtained.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
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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 10297-05-9 as follows. Recommanded Product: 10297-05-9

3.98 1-(4-Chlorobutyl)-13-dihydrobenzoimidazol-2-one (56NK92) Sodium hydride (400 mg, 10 mmol, 60percent in oil) was washed with dry DMF (10 ml) under an argon atmosphere then DMF (10 ml) was added. The slurry of NaH in DMF was added slowly to 2-hydroxybenzimidazole (1.34 g, 10 mmol) in DMF (10 ml) at 0° C. under argon. The reaction was stirred at 0° C. for 20 min then 1-chloro-4-iodobutane (2.18 g, 10 mmol) in DMF (5 ml) was added slowly. The reaction was stirred at r.t. for 1.5 h then water (10 ml) was added and the reaction acidified with HCl (2M, few drops) then made basic with aqueous sodium hydrogen carbonate solution. The product was extracted with EtOAc (3*30 ml) and the organic layer was washed with aqueous sodium thiosulphate solution (10 ml), aqueous magnesium sulphate solution (4percent, 2*10 ml), brine (10 ml), dried (K2CO3), filtered and concentrated in vacuo before being purified by using an Isco CombiFlash Sq 16x [10 g silica column, eluding heptane (5 min), 0-40percent EtOAc in heptane (35 min), 40percent EtOAc in heptane (20 min)] to give the title compound (56NK92) as a pale yellow oil (416 mg, 19percent). 1H NMR (CDCl3) delta 10.48 (br. s, 1H), 7.26-7.00 (m, 4H), 3.95 (t, J=6.8 Hz, 2H), 3.59 (t, J=6.3 Hz, 2H), 1.97 (m, 2H), 1.87 (m, 2H); 13C NMR (CDCl3) delta 158.88, 130.08, 128.14, 121.56, 121.25, 109.82, 107.74, 44.32, 39.88, 29.53, 25.66; HPLC-MS (ammonium acetate) [M+H]+=225.2.

According to the analysis of related databases, 10297-05-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kelly, Nicholas Michael; Koch, Kristian Norup; Tolf, Bo-Ragnar; US2004/67931; (2004); A1;,
Iodide – Wikipedia,
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Related Products of 41252-96-4, The chemical industry reduces the impact on the environment during synthesis 41252-96-4, name is 2-Chloro-1-iodo-4-nitrobenzene, I believe this compound will play a more active role in future production and life.

(i) Ethyl (2-chloro-4-nitrophenyl)(methyl)phosphinate To a solution of ethyl methylphosphinate (see, for example, Chebib, M. et al., WO 2006/000043, 5 January 2006; 530 mg, 4.90 mmol) in toluene (5 ml_) were added 2-chloro-1- iodo-4-nitrobenzene (835 mg, 2.95 mmol) and DIPEA (1.5 ml_, 8.59 mmol). The mixture was degassed under vacuum and back filled with nitrogen three times. XantPhos G3 precatalyst (84 mg, 0.088 mmol) was added, and the mixture was degassed three more times. The reaction was heated at 100C (block temperature) under nitrogen for 1 h. The reaction was cooled and the solvent evaporated to give a brown gum. The resulting gum was dissolved in DCM (30 ml_), 1 M HCL (20 ml_) was added and the phases were seperated. The organic phase was dried (MgSCU) and concentrated under reduced pressure. The crude material was purified by chromatography on silica gel (12 g column, dry load, 50-100% EtOAc/isohexane, product eluted at 98%) to afford the sub-title compound (519 mg) as a brown solid. 1 H NMR (400 MHz, DMSO-d6) delta: 8.40 (dd, 1 H), 8.35 (ddd, 1 H), 8.23 (dd, 1 H), 4.00 (ddq, 1 H), 3.83 (ddq, 1 H), 1.85 (d, 3H), 1.23 (t, 3H). LCMS m/z 264 (M+H)+ (ES+)

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-Chloro-1-iodo-4-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RESPIVERT LIMITED; TOPIVERT PHARMA LIMITED; BAKER, Thomas Matthew; FYFE, Matthew Colin Thor; JONES, Geraint; THOM, Stephen Malcolm; (270 pag.)WO2016/51187; (2016); A1;,
Iodide – Wikipedia,
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Synthetic Route of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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.

General procedure: Aryl iodide or bromides (1 mmol), ArOH (1 mmol), CuI(20 mol%), and dimethyl di (2-pyridyl)silane (20 mol%) were placed in a small round-bottom flask. DMF (3 mL) and K2CO3(276 mg, 2 mmol) were then added together. The mixture was stirred for 24 h at 100C in nitrogen atmosphere. The reaction mixture was cooled to room temperature. Ethyl acetate(10 mL) and H2O (1 mL) were added and the mixture was stirred. The organic layer was separated and the aqueous layer was extracted twice more with ethyl acetate (10 mL). Combined organic layer was dried overNa2SO4 and filtered. The filtrate was concentrated and the resulting residue was purified by silica gelchromatography and afforded the desired products.

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Baohua; Shi, Lanxiang; Guo, Ruixia; Liu, Sijie; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 6; (2016); p. 930 – 932;,
Iodide – Wikipedia,
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Synthetic Route of 5471-81-8, The chemical industry reduces the impact on the environment during synthesis 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, I believe this compound will play a more active role in future production and life.

(a) Synthesis of methyl 3-methyl-4-(3-ethyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyloxy)benzoate In a manner similar to Example 1(a), by the reaction of 2.1 g (8.7 mmol) of 3-ethyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthol with 2 g (7.2 mmol) of methyl 3-methyl-4-iodobenzoate, 2.18 g (79%) of the expected methyl ester was obtained in the form of a pale yellow oil.

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, Methyl 4-iodo-3-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Centre International de Recherches Dermatologiques Galderma; US6162815; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 6940-76-7, name is 1-Chloro-3-iodopropane, 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 6940-76-7, HPLC of Formula: C3H6ClI

A reaction flask or vial was charged 4H-benzo[1,4]ox- azin-3-one (1.0 equiv) dissolved in DMF (0.1 g/ml), Cs2CO3(1.5 equiv) and 1 -chloro-3-iodopropane (1.1 equiv). The reaction was stirred in rt for 60-70 h and evaporated to dryness. The reaction was redisolved in H20 and extractedwith EtOAc 3×1 50 ml. The combined organic phases weredried over Na2SO4 and concentrated to a crude that was useddirectly or purified by column chromatography (heptanes/ EtOAc).5,7-Difluoro-4H-benzo[ 1 ,4]oxazin-3-one (0.24 g, 1.3 mmol), Cs2CO3 (1.08 g, 3.3 mmol), and 1-chloro-3-iodo- propane (0.296 g, 1.45 mmol) were mixed according to GP2.Purified by column chromatography (Si02 heptanes/ EtOAc, gradient 0 to 30% EtOAc) to give the title compound (0.17 g, 49%). R1=0.66 (heptanes/EtOAc 1:1); ?H NMR (CDC13) oe 6.67-6.58 (m, 2H), 4.55 (s, 2H), 4.16-4.10 (m, 2H), 3.59-3.52 (m, 2H), 2.21-2.10 (m, 2H).

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-Chloro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ACADIA PHARMACEUTICALS, INC.; Skjaerbaek, Niels; Koch, Kristian Norup; Friberg, Bo Lennart Mikael; Tolf, Bo-Ragnar; (70 pag.)US9522906; (2016); B2;,
Iodide – Wikipedia,
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Electric Literature of 19099-54-8, A common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, molecular formula is C9H11I, 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.

Cu (I) iodide (38 mg, 0.2 mmol) and potassium carbonate (276 mg, 2.0 mmol) were charged into a screw-capped test tube with Teflon-lined septum. The tube was evacuated and backfilled with argon (3 cycles). tert-Amyl alcohol (2-methyl-2-butanol) (1.0 [ML,] bench grade solvent without degassing and pre-drying), ethylene glycol [(111 GL,] 2.0 mmol, bench grade solvent), 2-isopropyliodobenzene (246 mg, 1.0 mmol) and 2- isopropylbenzenethiol (90% purity, 202 muL, 1.2 mmol) were added by syringes at room temperature. The tube was heated to [100 C] and stirred for 24 hours. The reaction mixture was then allowed to reach room temperature. Ethyl acetate (approx. 5 mL) and dodecane (227 [FIL,] GC standard) were added. The aliquot was analyzed GC. The reaction mixture was then filtered and concentrated. The crude product was purified by column chromatography on silica gel using hexane as eluent to afford colorless oil as the titled product (245 mg, 91% yield). Rf= 0.5 [(HEXANE).’H] NMR (CDC13,300 MHz) 8 7.30 (d, 2 H, [J =] 7.2 Hz), 7.18-7. 24 (m, 2 H), 7.03-7. 05 (m, [4] H), 3.50 (hept, 2 H, J = 6.9 Hz), 1.25 (s, 3 H), 1.23 (s, [3 H). 13C NMR (CDC13,] 75 MHz) 6 149.2, 134.2, 132.1, 127.6, 126.7, 125.9, 30.9, 23.8. IR (neat, [CM”)] 3058,2962, 2929,2867. MS [(EI)] [FILZ] (relative intensity) 270 (100), 211 (90). HRMS [(EI),] Cald. for [CIUSDH22S] 270.1442 ; Found 270.1445.

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; MASSACHUSETTS INSTITUTE OF TECHNOLOGY; WO2004/13094; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 16932-44-8, 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. 16932-44-8 name is 2-Iodo-1,3-dimethoxybenzene, 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.

at -30 add isopropyl magnesium chloride (2.0M, 5.0mL, 10.0mmol) in THFTo compound 4 (2.64g, 10.0mmol) in anhydrous THF solution (30mL). The temperature was raised to 15 Thereafter, the mixture was stirred for 1 hour. The reaction solution was cooled to -78 , and phosphorus trichloride (0.69g,5.0mmol) were added thereto. At -78 deg.] C the resulting mixture was stirred for 1 hour. The solvent was removed under reduced pressure,To obtain a compound 5.

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

Reference:
Patent; Japan Polypropylene Corporation; Tanna, Akirahisashi; Sato, Naomasa; Konishi, Yohei; Oishi, Yasuo; (27 pag.)CN105593235; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 19099-54-8, 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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

l-Iodo-2-isopropylbenzene (1.5 g, 6.1 mmol) was suspended with silver sulfate (1.0 g, 3.1 mmol), concentrated sulfuric acid (5.5 mL), water (0.6 mL), and bromine (0.3 mL, 6.4 mmol). The triphasic solution was stirred at room temperature for 1 h. The mixture was poured into ether (150 niL) and water (75 rnL). The solids were filtered and the layers separated. The organic layer was concentrated in vacuo and the residue purified by preparatory HPLC to afford the title compound as a white solid (189 mg, 10%).[0257] 1H NMR (500 MHz, DMSO-J6) delta 1.18 (d, J = 6.8 Hz, 6H), 3.07 (qn, J = 6.8 Hz, IH), 7.15 (dd, J = 8.4, 2.5 Hz, IH), 7.46 (d, J = 2.4 Hz, IH), 7.75 (d, J= SA Hz, IH) 2D NOE (500 MHz, DMSO-J6): crosspeak between delta 1.18 and 7.46

The synthetic route of 1-Iodo-2-isopropylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TARGEGEN INC.; WO2009/55674; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 19094-56-5, 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: The 25-OCH3-PPD (1 equiv) was added to a solution of DCC (2 equiv), DMAP (0.2 equiv) and different aromatic groups (1 equiv) in dry dichloromethane and the reaction mixtures were shaken for 24 h. The solvent was removed under reduced pressure to give a white solid. The white solid was dissolved in ethyl ether and washed with NaHCO3 (5%), dried (MgSO4) and concentrated under reduced pressure to give the crude product. The crude products were chromatographed by silica gel and eluted with petroleum ether/ethyl acetate (4:1, 2:1 and 1:1) to give the pure products 1b, 1c and 1a. Using the same procedure described above for the other compounds.

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-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Qu, Fan-Zhi; Xiao, Sheng-Nan; Wang, Xu-De; Zhang, Yan; Su, Guang-Yue; Zhao, Yu-Qing; Bioorganic and Medicinal Chemistry Letters; vol. 29; 2; (2019); p. 189 – 193;,
Iodide – Wikipedia,
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