Category: 452-82-4

Electric Literature of 452-82-4,Some common heterocyclic compound, 452-82-4, name is 1-Fluoro-2-iodo-4-methylbenzene, molecular formula is C7H6FI, 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.

9A. 4-Bromomethyl-1-fluoro-2-iodo-benzene 4-Fluoro-3-iodotoluene (50 g, 210 mMol), N-bromosuccinimide (37.7 g, 212 mMol) and 2,2′-azobis-(2-methylpropionitrile) (348 mg, 2.12 mMol) were dissolved in carbon tetrachloride (300 mL) under an atmosphere of dry N2. The mixture was heated to reflux for 4 hours and then cooled to ambient temperature. The mixture was concentrated under vacuum and triturated with Et2 O. The filtrate was successively washed with water, aqueous saturated NaHCO3 and brine. The ether layer was dried over MgSO4, filtered and concentrated under vacuum to give a red oil. The oil was chromatographed on flash silica gel eluding with hexanes to give 33.8 g of the titled compound as a white solid.

The synthetic route of 452-82-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Inc.; US6150377; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 452-82-4,Some common heterocyclic compound, 452-82-4, name is 1-Fluoro-2-iodo-4-methylbenzene, molecular formula is C7H6FI, 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.

Example 8A 4-fluoro-3-iodobenzaldehyde A mixture of 4-fluoro-3-iodotoluene (5.0 g, 21.2 mmol) and NBS (4.2 g, 23.3 mmol) in 50 mL of CCl4 was refluxed under N2 with benzoyl peroxide (250 mg, 1.03 mmol) was heated for 3 hours. The reaction mixture was cooled to room temperature and filtered through celite, washed with benzene. The filtrate was evaporated and pumped to give the benzylbromide as a crude light brown oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Fluoro-2-iodo-4-methylbenzene, its application will become more common.

Reference:
Patent; Xin, Zhili; Liu, Gang; Pei, Zhonghua; Szczepankiewicz, Bruce G.; Serby, Michael D.; Zhao, Hongyu; US2004/167188; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 452-82-4,Some common heterocyclic compound, 452-82-4, name is 1-Fluoro-2-iodo-4-methylbenzene, molecular formula is C7H6FI, 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.

Example 2: 4-(Bromomethyl)-l-fluoro-2-iodobenzene Int-10 Step 1: 4-(Bromomethyl)-l-fluoro-2-iodobenzene Int-10 A mixture of 4-fluoro-3-iodotoluene (5 g, 21 mmol), NBS (3.77 g, 21 mmol) and azobisisobutyronitrile (35 mg, 0.21 mmol) in CC14 (30 mL) was heated to reflux for 4 h. The reaction was cooled to rt and concentrated. The residue was purified on silica gel to obtain 4-(bromomethyl)-l-fluoro- 2-iodobenzene (1.7 g, 26%). ‘HNMR (CDC13) delta 7.78 – 7.80 (m, IH), 7.32 – 7.37 (m, IH), 7.00 – 7.05 (m, IH), 4.41 (s, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Fluoro-2-iodo-4-methylbenzene, its application will become more common.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; DUFFEY, Matthew, O.; ENGLAND, Dylan, B.; HU, Zhigen; ITO, Mitsuhiro; LANGSTON, Steven, P.; MCINTYRE, Charles; MIZUTANI, Hirotake; XU, He; WO2015/2994; (2015); A2;,
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 452-82-4 as follows. Formula: C7H6FI

A mixture of 4-fluoro-3-iodotoluene (5.0 g, 21.2 mmol) and NBS (4.2 g, 23.3 mmol) in 50 mL of CCl 4 was refluxed under N 2 with benzoyl peroxide (250 mg, 1.03 mmol) was heated for 3 hours. The reaction mixture was cooled to room temperature and filtered through celite, washed with benzene. The filtrate was evaporated and pumped to give the benzylbromide as a crude light brown oil. [0192] A mixture of benzylbromide in 50 mL of DMSO was heated with NaHCO 3 solid (3.55 g, 42.2 mmol) at 120¡ã C. for 90 min. The reaction mixture was then cooled to room temperature, quenched with water, extracted with Et 2O, and washed with water, brine. The organic layer was dried with Na 2SO 4, concentrated in vacuuo. MPLC purification provided the titled compound as a colorless oil which solidified over time (2.2 g, 41.5% over two steps).

According to the analysis of related databases, 452-82-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Xin, Zhili; Liu, Gang; Pei, Zhonghua; Szczepankiewicz, Bruce G.; Serby, Michael D.; Zhao, Hongyu; US2004/214870; (2004); 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. 452-82-4, name is 1-Fluoro-2-iodo-4-methylbenzene, A new synthetic method of this compound is introduced below., 452-82-4

General procedure: A sealed tube equipped with a magnetic stir bar was charged with the corresponding 1-bromo -2-fluoro (or chloro) benzene/ 1-fluoro-2-iodobenzene (1 mmol), amino phenol (1 mmol), Pd(OAc)2 (5 mol%), xantphos (5 mol%) and DBU (2.5 mmol). The tube was purged with argon. Then DMF (10 V) was added followed by the addition of Co2(CO)8 (0.25 mmol). The tube was closed with seal plug instantly. The reaction tube was placed in a pre heated oil bath at 150 0C for 16 h. On completion, the reaction mixture was cooled to room temperature, added water and ethyl acetate (1:1). Precipitated solid was filtered through a Celite bed. The bed was washed thoroughly with ethyl acetate. Organic layer was separated. Aqueous layer extracted with EtOAc. The combined organic layers were washed with water, brine, dried over anhydrous sodium sulphate. Organic layer was concentrated under reduced pressure and purified by flash column chromatography on silica gel (230-400 mesh) with ethyl acetate and petroleum ether as eluent to afford the corresponding dibenzoxazepinones.

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; Anchan, Kavitha; Baburajan, Poongavanam; Puttappa, Nagaswarupa H.; Kumar Sarkar, Sujit; Synthetic Communications; vol. 50; 3; (2020); p. 348 – 360;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com