Tag: M.W=400-500

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 63262-06-6 as follows. 63262-06-6

To a solution of 1,4-dibromo-2,5-diiodo-benzene (15.0 g, 31 mmol) and ethynyl-trimethyl-silane (6.0 g, 62 mmol) in tetrahydrofuran (150 cm3) under nitrogen atmosphere at room temperature is added diisopropylamine (90 cm3, 640 mmol), copper(I)iodide (353 mg, 1.9 mmol) and bis(triphenylphosphine) palladium(II)chloride (60 mg, 0.9 mmol). The resulting mixture is stirred at 23 C for 17 hours, poured into water (100 cm3) and extracted with diethyl ether (5¡Á50 cm3). The combined organic layer is washed with water (50 cm3), brine (50 cm3) and dried over anhydrous magnesium sulfate then filtered. The filtrate is concentrated in vacuo to obtain an oily residue. The crude is purified using silica gel column chromatography (40-60 petroleum) to obtain an oily residue. The resulting oil is triturated with methanol to form a fine cream precipitate, which was filtered and washed well with methanol to give 1,4-dibromo-2,5-bis-trimethylsilanylethynyl-benzene (11 g, 84%) as a cream solid.

According to the analysis of related databases, 63262-06-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; Mitchell, William; D’Lavari, Mansoor; Wang, Changsheng; Tierney, Steven; Song, Jingyao; (75 pag.)KR2015/16254; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 63262-06-6 name is 1,4-Dibromo-2,5-diiodobenzene, 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. 63262-06-6

9.75 g of compound 3 and 0.562 gBis(triphenylphosphine)palladium dichlorideAnd 2-tributylstannylthiophene was dissolved in 70 mL of toluene.Stirring at 80 C for 2 days,It was then cooled to room temperature.Remove all liquids by rotary evaporator.The residue was recrystallized from methanol to give 5.6 g of Compound 4.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,4-Dibromo-2,5-diiodobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Chinese Academy Of Sciences Ningbo Materials Technology And Engineering Institute; Ge Ziyi; Xie Lingchao; Xiao Jingbo; Huang Jiaming; Peng Ruixiang; (23 pag.)CN109970761; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

63262-06-6, A common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, molecular formula is C6H2Br2I2, 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: In argon atmosphere, Pd(PPh3)2Cl2(115 mg, 0.164mmol) and CuI (156 mg, 0.820 mmol) were added to a stirring solutionof CuI (4.00 g, 8.20 mmol) in anhydrous THF/Et3N (30 ml, 1/1). 4-Ethyloct-1-yne(2.49 g, 18.0 mmol) was then added with a syringe. Theresulting mixture was stirred overnight at room temperature, and then pouredinto a large amount of dilute ammonia water for extraction with petroleum ether.The combined organic extracts were washed with saturated NH4Claqueous solution and brine until to neutral, dried over anhydrous MgSO4and concentrated in vacuum. The residue was purified with column chromatographyon silica gel with petroleum ether as the eluent

The synthetic route of 63262-06-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shao, Jing; Zhao, Xiaoli; Wang, Li; Tang, Qingxin; Li, Weili; Yu, Han; Tian, Hongkun; Zhang, Xiaojie; Geng, Yanhou; Wang, Fosong; Tetrahedron Letters; vol. 55; 41; (2014); p. 5663 – 5666;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com